WO2019048715A2

WO2019048715A2 - Compositions containing activated pectin-containing biomass composition, and methods of manufacturing such compositions

Info

Publication number: WO2019048715A2
Application number: PCT/EP2019/050769
Authority: WO
Inventors: Ross C. Clark; Wencke Dybvik HENRIKSEN; Heidi Munck GRAVERSEN
Original assignee: Cp Kelco Aps
Priority date: 2018-01-16
Filing date: 2019-01-14
Publication date: 2019-03-14
Also published as: WO2019048715A3

Abstract

Provided are methods of expanding an activated pectin-containing biomass composition to form an expanded pectin-containing biomass composition, and compositions containing the activated pectin-containing biomass composition or the expanded pectin-containing biomass composition. The activated pectin-containing biomass composition and the expanded pectin-containing biomass composition contains pectin in an amount from at or about 20 wt% to at or about 50 wt%, and cellulosic fiber in an amount from at or about 80 wt% to at or about 50 wt%.

Description

COMPOSITIONS CONTAINING ACTIVATED PECTIN-CONTAINING BIOMASS COMPOSITION, AND METHODS OF MANUFACTURING SUCH

COMPOSITIONS

FIELD

The present invention relates generally to pectin-containing biomass compositions, methods for the manufacture of the pectin-containing biomass compositions, and products containing the pectin-containing biomass compositions. The pectin-containing biomass compositions are useful as a thickener, texturizer, stabilizer, in foods and beverages, cosmetics, personal care products, household care products, detergents, nutraceuticals, pharmaceuticals, toothpastes, filter media, and as an additive, e.g., for paper, paper coatings, non-woven materials, fracturing fluids, casing milling operations, gravel packing, spacer fluids, cementing, surfactants, ceramics for porosity modification, flocculation, sealants and caulks, printing inks, friction material, and protective coatings. Further the pectin-containing biomass compositions may provide enhanced mouthfeel for no or reduced fat and sugar foods or beverages and may be used as an alternative to starch or egg yolk.

BACKGROUND

There is an increasing demand for more natural materials for use as rheology and texture modifiers in food, pharmaceutical and industrial applications. Use of cellulose fiber-based materials in these application has increased during the last decade. For example, U.S. Pat. App. Pub. No. US2014/0363560 (Lundberg, 2014) describes hydrocolloids co-processed with cellulosic fibers when sheared into refined cellulose as a cellulose fiber material that can be used as a thickener.

Citrus fiber is a cellulose fiber that traditionally was viewed to be a waste byproduct from the production of pectin, and its major use was as a feed for livestock. Methods of producing pectin from plant products are known in the art. For example, see U.S. Patent Nos. 2,132,065 (Wilson, 1938); 2,452,750 (Halliday, 1948); 2,550,705 (Maclay et al, 1951); 2,577,232 (Cole, 1951); 2,647,890 (Bishop, 1953); 2,801,178 (Leo et al, 1957); 3,622,559 (Wiles et al, 1971); 3,982,003 (Mitchell et al, 1976); 4,143,172 (Mitchell et al, 1979); 4,686,187 (Sakai et al, 1987); 4,831,127 (Weibel, 1989); 4,923,981 (Weibel et al, 1990); 5,071,970 (le Grand et al, 1991); 5,567,462 (Ehrlich, 1996); 6,143,337 (Fishman et al, 2000); 6,143,346 (Glahn, 2000); 6,183,806 (Ficca et al, 2001); 6,207,194 (Glahn, 2001); 6,855,363 (Buchholt et al, 2005); 7,094,317 (Lundberg et al, 2006); 7,691,986 (Ni et al, 2010); and 8,592,575 (Jensen et al, 2013). These methods tend to focus on the complete or maximum removal of pectin from pectin-containing materials, leaving only cellulosic citrus fiber material mostly devoid of pectin as the by- product.

Prior art methods for preparing cellulose fiber from plant materials are known. For example, U.S. Pat. No. 3,023,104 (Baltista, 1962) describes preparation of cellulose crystallite aggregates by subjecting cotton, bleached sulfite pulp, or bleached sulfate wood pulp to acid hydrolysis and mechanical disintegration of the fibers. U.S. Pat. No. 4,307,121 (Thompson, 1981) describes a process for producing a cellulosic product suitable for human consumption that includes subjecting ground soy hulls, yellow field pea hulls, or corn bran to multiple oxidation conditions with chlorine gas and separating the treated short fiber cellulose. U.S. Pat. No. 4,923,981 describes the preparation of parenchyma cell cellulose from pectin-containing materials, such as sugar beet and citrus pulp. The materials are first treated with a strong acid or a strong base at high temperatures for short periods of time to release the cellulosic and hemi-cellulosic components thereof. The treatment releases pectin from the starting materials without substantial degradation. The starting material is subjected to physical shearing, and the solid (cellulose-containing) fraction and liquid (pectin-containing) fraction of the treated mixture are separated and used separately. Cellulose fibrillation is known in the art {e.g., see U.S. Pat. No. 8,915,457, Dodd et al, 2014).

While the prior art reports that some of the cellulose fiber obtained from such processes can exhibit useful properties, there remains a need to further improve the functionality of the fiber. Additionally, the processes for producing fiber can be improved to yield an improved fiber that can exhibit more functional properties than demonstrated by the by-product of the pectin production processes.

SUMMARY

Accordingly, it is an object of the present invention to provide a pectin-containing biomass composition that exhibits improved rheology modifying properties.

U.S. Provisional Patent Application Ser. No. 62/459,136 and U.S. Patent Application Ser. No. 15/892,639 both to Staunstrup et al. (hereinafter referred to as "Staunstrup Applications") disclose an activated pectin-containing biomass composition prepared by treating a starting pectin-containing biomass composition with an activating solution comprising an alcohol and an acid (further defined below) to form a mixture and exposing the mixture to heat and a certain amount of mechanical energy under non- laminar flow to transform insoluble protopectin to soluble pectin in situ and to partially fibrillate a portion of the cellulosic fibers into fibrils, thus providing for a final composition with increased apparent viscosity and water binding characteristics and a high ratio of soluble pectin to insoluble fiber. Provided herein are compositions that contain the activated pectin-containing biomass composition.

Also provided are methods of expanding the activated pectin-containing biomass composition to yield an expanded pectin-containing biomass composition. It has surprisingly been found that exposing the activated pectin-containing biomass composition to an extensional stress results in a product demonstrating improved rheological properties. The methods include mixing an activated pectin-containing biomass composition with a fluid to form a mixture, and subjecting the mixture to an extensional stress, where a) the activated pectin-containing biomass composition has a coil overlap parameter of 2 or greater; or b) the activated pectin-containing biomass composition has an apparent viscosity from about 150 mPa*s to about 3500 mPa*s when measured in aqueous solution at a temperature of 25 °C and a pH of 4.0; or c) the activated pectin- containing biomass composition comprises pectin in an amount from at or about 20 wt% to at or about 50 wt%, and cellulosic fiber in an amount from at or about 80 wt% to at or about 50 wt%; or d) the activated pectin-containing biomass composition is substantially free of D-limonene; or e) any combination of a), b), c) and d). The extensional stress can be applied to the mixture using any device that can produce turbulent flow. Examples of such devices include propeller mixers, rotor stator mixing devices, such as a Silverson mixer, a toothed-ring disperser, an annular-gap mill or a colloid mill, and homogenizers, such as a high pressure homogenizer, a microfluidizer, a French press homogenizer, and an extensional homogenizer, or any combination thereof. A propeller mixer exerts less extensional stress than a rotor stator mixer, and a rotor stator mixer exerts less extensional stress than a homogenizer. The extensional stress can be applied to the mixture using a homogenizer, such as a high pressure homogenizer. Exemplary high pressure homogenizers include an Avestin homogenizer, a BEE homogenizer, a counter flow homogenizer, an extensional homogenizer, a Gaulin homogenizer, a Niro homogenizer, and a Rannie homogenizer. The high pressure homogenizer can be operated at a pressure of at least 3,000 psi. The fluid can be aqueous or non-aqueous. The fluid can be at least a portion of a liquid component of a composition comprising the liquid component and one or more ingredients. The one or more ingredients of the composition can be added to the mixture prior to subjecting the mixture to an extensional stress. The one or more ingredients of the composition can be added to the mixture after subjecting the mixture to an extensional stress.

Also provided is an expanded pectin-containing biomass composition produced by the methods described herein. The expanded pectin-containing biomass composition can exhibit a synergistic interaction with a protein. The protein can be a plant-based protein, egg white, sodium caseinate, milk protein or a whey protein. The expanded pectin- containing biomass composition can exhibit a synergistic interaction with a hydrocolloid. The hydrocolloid can be a starch, a xanthan gum, a pectin or a combination thereof. The expanded pectin-containing biomass composition can produce a thickened aqueous composition containing 0.25% of the expanded pectin-containing biomass composition having a viscosity of at least at or about 500 mPa*s at 3 rpm on a Brookfield viscometer.

Also provided are compositions that include from at or about 0.01 wt% to at or about 2 wt% of the expanded pectin-containing biomass composition provided herein, or from at or about 0.01 wt% to at or about 5 wt% of an activated pectin-containing biomass composition having a coil overlap parameter of 2 or greater. The composition can be a food, industrial, oilfield, pharmaceutical, nutraceutical, dermato logical, cosmetic, household care, or personal care product. The composition can be a stirred or drinkable yogurt fruit or/vanilla preparation, a salad dressing, a preserve, a jam, a jelly, a low sugar or no-sugar added fruit spread, a fruit pie filling, a fruit concentrate for ice cream manufacturing, an ice cream topping, a fruit leather, a sorbet, a dairy dessert, an ice cream, an ice milk, a plant-based non-dairy dessert, a water ice, a pudding, a custard, a mayonnaise, a low- fat or non-fat mayonnaise, a margarine, a low- fat spread, a sour cream, a low fat or non-fat sour cream, a peanut butter, a nut spread, a vanilla or chocolate spread, an extruded snack, a soup, a sauce, a gravy, a marinade, a carbonated beverage, an energy drink, a fruit juice, a vegetable juice, a cocoa-based beverage, a caramel or chocolate syrup, a dairy beverage, a chocolate milk, a beverage concentrate, an acidified protein drink, a drinkable yogurt, a yogurt, a whipped yogurt, a cheese spread, a processed cheese, a batter, a coating, film former, a liquid fond concentrate, a bouillon, a whipped topping, a marshmallow product, a confection product, a whipped confection product, a candy, a toothpaste, a dental rinse, a ketchup, a barbeque sauce, a dysphagia product, a breakfast cereal, a baked good, a pastry, a cake, a patisserie, a cookie, a pie crust, a bread, a cracker, a dough, cereal snack/granola a thermostable filling having a low or ultra-low water activity, a dairy product, a meat additive, a meat extender, a paper, a paper coating, a nonwoven, a specialty laid sheet, a dielectric sheet, a battery separator, a capacitor separator, a fracturing fluid, a drilling mud, a weighted or inhibited fluid for oilfield applications, a gravel packing composition, a cementing formulation, a spacer fluid, a pore former in a ceramic or catalyst composition, a flocculation medium, a fining agent, a filter medium, a tub or tile cleaner, a hard surface cleaner, a dish detergent, a floor cleaner, a carpet cleaner, a sanitizer, a wood and furniture polish, a toilet bowl cleaner, an antifog agent, a drain cleaner, a scale remover, a paint, a paint remover, a stain, a stain remover, a dye, a printing ink, a nutraceutical, a pharmaceutical elixir, a suspension, a syrup, a tablet binder, a tablet disintegrant, a pet product, an animal feed product, a shampoo, a conditioner, a cream, a styling gel, a sun screen, a hand or body lotion, a fabric detergent, a high surfactant laundry detergent, a fabric conditioner, a wax suspension, a weed control composition, or an agricultural emulsion.

When the composition is a food product, the expanded pectin-containing biomass composition, or the activated pectin-containing biomass composition, can replace at least a portion of a fat or a carbohydrate or both in the food product, resulting in a reduced calorie content or a reduced fat content or both. The inclusion of the expanded pectin-containing biomass composition, or the activated pectin-containing biomass composition, can result in a product having an improved texture, an improved mouthfeel or an improved flavor release compared to a comparable food product in which the expanded pectin-containing biomass composition or activated pectin-containing biomass composition is not present. The food product can be an emulsion, a foam, a batter or a dough. The inclusion of the expanded pectin-containing biomass composition, or the activated pectin-containing biomass composition, can a) suspend particulates in the composition; or b) minimize coalescence of fat globules in the composition; or c) minimize coalescence of air bubbles in the composition; or d) any combination of a), b) and c).

The composition containing the expanded pectin-containing biomass composition, or the activated pectin-containing biomass composition, can be a pharmaceutical, cosmetic, dermato logical or personal care product, and further include an active ingredient.

Also provided are methods for modifying a rheo logical property of a composition. The methods include adding to the composition an amount of the expanded pectin- containing biomass composition provided herein, or an activated pectin-containing biomass composition having a coil overlap parameter of 2 or greater, sufficient to increase the viscosity, or to modulate the yield stress of the composition. The composition can be a food, industrial, pharmaceutical, nutraceutical, cosmetic, oilfield, household care, or personal care product.

Also provided are methods for altering a physical or processing property of a composition. The methods include adding to the composition an amount of the expanded pectin-containing biomass composition provided herein, or an activated pectin-containing biomass composition having a coil overlap parameter of 2 or greater, sufficient to alter a physical property or processing property of the composition. The composition can be a food, industrial, pharmaceutical, nutraceutical, dermato logical, cosmetic, oilfield, household care, or personal care product. The method can include exposing the composition to an extensional stress after the expanded pectin-containing biomass composition, or the activated pectin-containing biomass composition having a coil overlap parameter of 2 or greater, is added to the components. The extensional stress can be applied by passing the composition through a high pressure homogenizer. The composition can be passed through the high pressure homogenizer at least 2 times. The high pressure homogenizer is operated at a pressure of at least 3,000 psi. The composition can be a yogurt fruit preparation, a salad dressing, a preserve, a jam, a jelly, a low sugar or no-sugar added fruit spread, a fruit pie filling, a fruit concentrate for ice cream manufacturing, an ice cream topping, a fruit leather, a sorbet, a dairy dessert, an ice cream, an ice milk, a non-dairy dessert, a water ice, a pudding, a custard, a mayonnaise, a low-fat or non-fat mayonnaise, a margarine, a low-fat spread, a sour cream, a low fat or non-fat sour cream, a peanut butter, a nut spread, a chocolate spread, an extruded snack, a soup, a sauce, a gravy, a marinade, a carbonated beverage, an energy drink, a fruit juice, a vegetable juice, a cocoa-based beverage, a chocolate syrup, a dairy beverage, a chocolate milk, a beverage concentrate, an acidified protein drink, a drinkable yogurt, a yogurt, a whipped yogurt, a cheese spread, a processed cheese, a batter, a coating, a whipped topping, a liquid fond concentrate, a bouillon, a whipped topping, a marshmallow product, a confection product, a whipped confection product, a candy, a toothpaste, a dental rinse, a ketchup, a barbeque sauce, a dysphagia product, a breakfast cereal, a baked good, a pastry, a cake, a patisserie, a cookie, a pie crust, a bread, a cracker, a thermostable filling having a low or ultra-low water activity, a dairy product, a meat additive, a meat extender, a paper, a paper coating, a nonwoven, a specialty laid sheet, a dielectric sheet, a battery separator, a capacitor separator, a fracturing fluid, a drilling mud, a weighted or inhibited fluid for oilfield applications, a gravel packing composition, a cementing formulation, a spacer fluid, a pore former in a ceramic or catalyst composition, a flocculation medium, a fining agent, a filter medium, a tub or tile cleaner, a hard surface cleaner, a dish detergent, a floor cleaner, a carpet cleaner, a sanitizer, a wood and furniture polish, a toilet bowl cleaner, an antifog agent, a drain cleaner, a scale remover, a paint, a paint remover, a stain, a stain remover, a dye, a printing ink, a nutraceutical, a pharmaceutical elixir, a suspension, a syrup, a tablet binder, a tablet disintegrant, a pet product, an animal feed product, a shampoo, a conditioner, a cream, a styling gel, a sun screen, a hand or body lotion, a fabric detergent, a high surfactant laundry detergent, a fabric conditioner, a wax suspension, a weed control composition, or an agricultural emulsion.

Also provided are methods for reducing the caloric content of a food product. The methods include replacing one or more of a fat, a sugar, or a starch or a portion thereof by adding an amount of the expanded pectin-containing biomass composition provided herein, or an activated pectin-containing biomass composition having a coil overlap parameter of 2 or greater, sufficient to yield a food product having commercially acceptable physical and processing characteristics.

Other objects, features and advantages of the compositions, systems and methods described herein will become apparent to those skilled in the art from the following detailed description. It is to be understood, however, that the detailed description, while indicating certain embodiments of the compositions and methods described herein, are given by way of illustration and not limitation. Many changes and modifications within the scope of the present invention may be made without departing from the spirit thereof.

DETAILED DESCRIPTION BRIEF DESCRIPTION OF THE FIGURES

The drawings described herein are for illustrative purposes only of selected embodiments and not all possible implementations, and are not intended to limit the scope of the present disclosure.

FIGS. 1A to 1C are electron micrographs of (A) expanded reticulated cellulosic fiber product provided herein; (B) expanded Fibergel LC product; and (C) expanded Ceamsa Ceamfibre. The micrographs are x3000 magnification. A. DEFINITIONS

Unless defined otherwise, all technical and scientific terms used herein have the same meaning as is commonly understood by one of skill in the art to which the inventions belong.

All patents, patent applications, published applications and publications, websites and other published materials referred to throughout the entire disclosure herein, unless noted otherwise, are incorporated by reference in their entirety. In the event that there are a plurality of definitions for terms herein, those in this section prevail. Where reference is made to a URL or other such identifier or address, it is understood that such identifiers can change and particular information on the internet can come and go, but equivalent information can be found by searching the internet. Reference thereto evidences the availability and public dissemination of such information.

As used here, the singular forms "a," "an" and "the" include plural referents unless the context clearly dictates otherwise.

As used herein, ranges and amounts can be expressed as "about" a particular value or range. "About" also includes the exact amount. Hence "about 5 percent" means "about 5 percent" and also "5 percent." "About" means within typical experimental error for the application or purpose intended. The term "about" can be used to mean, for example, within 10% of the recited value, within 5% of the recited value, or within 2% of the recited value.

As used herein, "optional" or "optionally" means that the subsequently described element, event or circumstance does or does not occur, and that the description includes instances where the element, event or circumstance occurs and instances where it does not. For example, an optional component in a system means that the component may be present or may not be present in the system.

In the examples, and throughout this disclosure, all parts and percentages are by weight (wt%) and all temperatures are in °C, unless otherwise indicated.

As used herein, the phrase "based on the weight of the composition" with reference to % refers to wt% (mass% or (w/w)%).

As used herein, "x and/or y" means x or y or both x and y.

As used herein, "starting pectin-containing biomass composition" refers to a fibrous pectin-cellulosic material obtained from a plant source. The plant source can be any of a wide variety of materials containing high levels of pectin, including citrus fruit, such as oranges, limes, lemons, grapefruit, pomelo, oroblanco and tangerines, as well as apple, pear, quince, grape, guava, pineapple, beet roots, chicory roots and carrots. The starting pectin-containing biomass composition can be a citrus pulp, a citrus peel, or a combination thereof.

As used herein, "reticulated" refers to a net-like arrangement or structure.

As used herein, "water holding" or "water binding" refers to the ability of a given solid to absorb water under static conditions.

As used herein, "activation" or "activated" refers to treating a starting pectin- containing biomass composition with an activating solution, heat and mechanical energy to hydro lyze the protopectin to yield a water-soluble pectin within the biomass and to at least partially fibrillate a portion of the cellulosic fibers into fibrils. Methods of preparing an activated pectin-containing biomass composition (also referred to herein as "activated PBC") are described in the Staunstrup Applications. Activated pectin-containing biomass composition in which citrus fruit is used as the raw material is herein after referred to as "activated citrus fiber".

As used herein, an "activating solution" refers to an alcohol solution containing an acid at a concentration sufficient to result in the activating solution having a pH of about 0.5 to 2.5 and sufficient to convert at least a portion of a protopectin into a pectin.

As used herein, "expanding" or "expansion" refers to the process of applying energy in the form of an extensional stress. The extensional stress results in expansion of the cellulosic network so that it is not compacted but instead cellulosic fibrils are physically separated and interact with other fibrils to form a reticulated web-like structure. Expanding allows the cellulosic fibers to increase their exposed surface area. The expanding does not have to be optimal to achieve maximum surface area of the cellulosic fiber for the expanded pectin-containing biomass composition to modify rheological or textural properties to a formulation or composition to which it is added. Any expanding of the activated pectin-containing biomass composition by exposure to an extensional stress can increase the exposed surface area of the cellulosic fibers and increase the efficiency of the expanded pectin-containing biomass composition to modify a rheological or textural property.

As used herein, an "expanded pectin-containing biomass composition" or

"expanded PBC" refers to an activated pectin-containing biomass composition, such as described in the Staunstrup Applications, that has been exposed to an extensional stress. Expanded pectin-containing biomass composition in which citrus fruit is used as the raw material is herein after referred to as "expanded citrus fiber". As used herein, a "co-agent" refers to a material that interferes with the natural tendency of cellulosic fibrils to associate. The most commonly used co-agent with some cellulosic fibers is carboxymethyl cellulose. The activated pectin-containing biomass composition sample fiber provided herein includes natural pectin components that can act as a co-agent for the cellulosic fibrils.

As used herein, the "coil overlap parameter" is determined by the following formula:

Coil Overlap Parameter = IV_pectin x Pectin Recovery, where the IVpectin is the intrinsic viscosity (IV) of the pectin extracted from the activated pectin-containing biomass composition, and the pectin recovery is the amount of pectin extracted from the activated pectin-containing biomass composition divided by the total amount of activated pectin-containing biomass composition.

As used herein, a "personal care product" refers to products intended for application to the human body, such as to skin, hair, and nails, including, but not limited to, shampoos, conditioners, creams, lotions, toothpaste, cosmetics, and soaps.

When a range of any type is described or claimed, the intent is to describe or claim individually each possible number that such a range could reasonably encompass, including end points of the range as well as any sub-ranges and combinations of subranges encompassed therein.

While compositions and methods are described herein in terms of "comprising" various components or steps, the compositions and methods can also "consist essentially of or "consist of the various components or steps, unless stated otherwise.

For the purposes of describing and defining the present teachings, the term "substantially" is used herein to represent the inherent degree of uncertainty that may be attributed to any quantitative comparison, value, measurement, or other representation. The term "substantially" is also used herein to represent the degree by which a quantitative representation may vary from a stated reference without resulting in a change in the basic function of the subject matter at issue.

B. METHODS FOR PRODUCING AN ACTIVATED PECTIN-CONTAINING

BIOMASS COMPOSITION

A detailed description of methods for preparing an activated pectin-containing biomass composition are described in co-pending, co-owned U.S. Patent Provisional Application Ser. No. 62/459,136, filed February 15, 2017, and U.S. Application Ser. No. 15/892639, filed February 9, 2018, which are incorporated herein by reference in their entirety. The process can use any high-pectin material as the starting pectin-containing biomass composition. For example, the starting pectin-containing biomass composition can be any pectin-containing biomass. The starting pectin-containing composition material can include an insoluble fiber component, which can be predominately hemicellulose and cellulose, as well as a protopectin (i.e. pectin in its insoluble form) component. Exemplary starting pectin-containing biomass compositions that can be used as a starting material includes, but is not limited to, citrus fruit or peel, such as orange peel, lemon peel, lime peel, grapefruit peel, pomelo peel, oroblanco peel, and tangerine peel, apple pomace, grape pomace, pear pomace, quince pomace, fodder beet, sugar beet, sugar beet residue from sugar extraction, sunflower residue from oil extraction, potato residue from starch production, Jerusalem artichokes, pineapple peel and core, and chicory roots.

The processes for preparation of activated pectin-containing biomass composition does not remove the natural pectic substances present in citrus peel. This results in an activated pectin-containing biomass composition that is not only highly functional, but also closer to nature, resulting in a minimally processed product.

When peels from a citrus fruit are used as a starting pectin-containing biomass composition, they can be used fresh or dried. The starting pectin-containing biomass composition can be washed and treated, such as to remove volatile oils. The starting pectin-containing biomass composition can be subjected to mechanical treatment to remove any residual wash water from the biomass. The starting pectin-containing biomass composition can be subjected to one or more solvent washes. The solvent can help to displace water from the biomass. The solvent can be an alcohol. The solvent can be a lower alcohol, such as ethanol or isopropanol, or a combination thereof. Subjecting the starting pectin-containing biomass composition to a solvent wash has been found to cause the protopectin in situ to lose its water binding ability, which results in water leaching out of the pectin-containing biomass composition without the protopectin, and therefore ultimately increasing pectin retention in the biomass composition.

The starting pectin-containing biomass composition can be a pectin-containing biomass composition prepared using the processes, in full or in part, as described in U.S. Patent No. 8,323,513 (Trudsoe et al., 2012), which is incorporated herein by reference. The starting pectin-containing biomass composition can be washed with an aqueous alcohol solution, having an alcohol content of at least 40% in order to remove solubles and harden the peel by making pectin and/or protopectin insoluble.

When the processes provided herein include a washing step, the washed material can be mechanically separated from at least a portion of the washing composition to form washed material. The mechanical separation can be done by draining, screening, decanting, centrifuging or pressing the washed material, which can be carried out using any suitable separation device. For example, a pressing device, such as a single screw press-type, can be used to separate the washed material from the washing liquid. In such instances, the pressure during pressing can range from about 0.5 bar to about 8 bar or from about 2 bar to about 4 bar, and the duration of the pressing can range from about 1 minute to about 25 minutes, or about 10 minutes to about 25 minutes, or about 15 minutes to about 25 minutes.

In the methods for producing an activated pectin-containing biomass composition, the starting pectin-containing biomass composition can be comminuted to reduce the size of the particles of the biomass. The biomass then can be dispersed in an activating solution, which is an acidic aqueous solution that includes water, an alcohol, and an acid, to form a mixture. The alcohol can be any C1-C4 alcohol, such as methanol, ethanol, isopropyl alcohol, butanol, or a combination thereof. The amount of alcohol present in the activating solution can be from at or about 40 wt% to at or about 80 wt% based on the weight of the activating solution. The activating solution can include an alcohol in an amount from at or about 40 wt% to at or about 60 wt% based on the weight of the activating solution. The activating solution can include an alcohol in an amount from at or about 50 wt% to at or about 60 wt% based on the weight of the activating solution. By keeping the amount of alcohol present in an amount of at least 40 wt%, the pectin produced can remain associated with the cellulosic fiber or be trapped within the network or both.

Any organic or inorganic acid can be included in the activating solution. Non- limiting examples of suitable acids include organic and inorganic acids such as nitric acid, hydrochloric acid, sulfuric acid, phosphoric acid, citric acid, oxalic acid, and combinations thereof. An acid commonly used in the production of pectin, such as nitric acid, can be used as the acid in the activating solution. The amount of acid present in the activating solution depends on the pKa of the acid. The amount of acid present in the activating solution is the amount necessary to achieve a pH of at or about 0.5 to at or about 2.5, or a pH of at or about 1.0 to at or about 2.0 in the mixture containing the biomass. The process can include addition of at or about 100 to at or about 200 mL concentrated (62%w/w) nitric acid per kg biomass (based on dry weight of the biomass). The process can include addition of at or about 150 mL concentrated nitric acid per kg biomass on a dry weight basis.

Prior to being subjected to the activating solution and mechanical energy, the starting pectin-containing biomass composition comprises the insoluble fiber component and protopectin. As the starting pectin-containing biomass composition, when in contact with the activating solution, is subjected to mechanical energy, the protopectin in the biomass, upon exposure to the acid, can hydrolyze in situ to yield a water soluble pectin within the biomass. The treatment results in an activated pectin-containing biomass composition that contains the insoluble fiber component (primarily cellulosic material) and the soluble pectin component. Not wishing to be bound by any theory, it is believed that the protopectin converts to water soluble pectin through the action of the acid and, due to the alcohol, does so without leaching out of the starting pectin containing biomass composition, a portion of the pectin becoming associated with the fibrils of the opened cellulosic structure produced by the exposure of the biomass to mechanical energy.

The mixture can be circulated in a closed-loop system that includes a pressure vessel (able to contain a heated solvent mixture), a reflux vessel, a heat exchanger, such as a shell and tube heat exchanger, and a pump for recirculating the heated mixture back to the vessel, allowing multiple passes through the pump in the system. Any pump that can exert a mechanical energy, such as a bi-axial extensional stress, on the fluid as it passes through the pump or through the system can be used. Examples include rotary lobe pumps (available from, e.g., Viking Pump, Inc., Cedar Falls, IA; Johnson Pump, Rockford, IL; and Wright Flow Technologies, Inc., Cedar Falls, IA); centrifugal pumps, and hydro- transport pumps (available from, e.g., Cornell Pump Company, Clackamas, OR; and Alfa Laval Inc., Richmond. VA). Other devices that can be used singularly or in combination to impart mechanical energy, such as a bi-axial extensional stress, include a plate refiner, a disc refiner, a hydropulper, an extruder, a friction grinder mill, a hammer mill, and a ball mill. Steam explosion or pressure relief also can be used to impact mechanical energy. The methods can be designed as continuous without circulating back to the pressure vessel.

The pump can be a rotary lobe pump, alone or in combination with another type of pump. The rotary lobe pump is a positive displacement pump and can have a single lobe, bi-wing, tri-lobe, or multi-lobe configuration. During operation, two rotors mesh together and rotate in opposite directions, forming cavities between the rotors and the housing of the pump. The mixture enters and fills the cavities, moving through the pump between the lobes and the casing. The movement of the lobes of the pump forces the mixture through the outlet port of the discharge side of the pump and the mixture is ejected from the pump. The movement of the mixture through the pump exposes the mixture to mechanical energy, which teases apart the cellulosic fibers at least partially into fibrils. The mechanical energy can include a bi-axial extensional stress. The lobe pump can continuously pump the mixture of comminuted peel through the heat exchanger and back to the tank or pressure vessel for a set time. The methods can be designed as continuous without circulating back to the tank or pressure vessel.

This mechanical energy imparted, such as by the action by the pump, which can induce turbulent flow within the pump and within the material as it is circulated through the closed-loop system or through the continuous process, opens the structure of the cellulosic component, visually changing the physical structure of the material as it takes on a more "fluffy" or "cotton-like" appearance when examined during the process. Turbulent flow leads to flow reversals and thus extension of the material within the mixture. The mechanical energy fibrillates at least a portion of the cellulosic fiber into fibrils, increasing the surface area and thus the efficacy of the cellulosic fibers.

The mechanical energy can include application of "high shear" to the material using the pump. The high shear energy, whether using a rotary lobe pump, a rotor stator mixer, a homogenizer or any combination thereof, is not intended to cut the cellulosic fibers, but instead to create a high Reynolds number that leads to flow reversals and thus application of extensional stress to the material, fibrillating the cellulosic fibers. The Reynolds number is a dimensionless value that measures the ratio of inertial forces to viscous forces and is useful for predicting flow patterns in a fluid, particularly the degree of turbulent or laminar flow. The Reynolds number can be calculated using Formula 1 :

Reynolds number = (fluid velocity * length scale) Formula 1

kinematic viscosity

Reynolds number values greater than 2500 are considered to have turbulence. For the processes provided herein, the parameters are adjusted to obtain a Reynolds number of at least 2500, such as by increasing the fluid velocity or increasing the length scale, either of which can induce more turbulent flows. High Reynolds numbers can lead to more fibrillated cellulosic fiber in a shorter period of time. Several parallel recirculating paths can be used to increase the exposure of the fluid mixture to extensional stress due to the turbulent flow.

The mechanical energy to achieve high turbulent flow by increasing fluid velocity can vary depending on the configuration of the system and can be expressed as energy consumption per weight of material. The mechanical energy can be at least 800 kJ/kg, or in the range of from about 800 to about 15,000 kJ/kg. The mechanical energy to which the mixture can be subjected can be at least any one of 800 kJ/kg, 1,000 kJ/kg, 1,200 kJ/kg, 1,400 kJ/kg, 1,600 kJ/kg, 1,800 kJ/kg, 2,000 kJ/kg, 2,200 kJ/kg, 2,400 kJ/kg, 2,600 kJ/kg, 2,800 kJ/kg, 3,000 kJ/kg, 3,200 kJ/kg, 3,400 kJ/kg, 3,600 kJ/kg, 3,800 kJ/kg, 4,000 kJ/kg, 4,200 kJ/kg, 4,400 kJ/kg, 4,600 kJ/kg, 4,800 kJ/kg, 5,000 kJ/kg, 5,200 kJ/kg, 5,400 kJ/kg, 5,600 kJ/kg, 5,800 kJ/kg, 6,000 kJ/kg, 6,200 kJ/kg, 6,400 kJ/kg, 6,800 kJ/kg, 7,000 kJ/kg, 7,200 kJ/kg, 7,400 kJ/kg, 7,600 kJ/kg, 7,800 kJ/kg, 8,000 kJ/kg, 8,200 kJ/kg, 8,400 kJ/kg, 8,600 kJ/kg, 8,800 kJ/kg, 9,000 kJ/kg, 9,200 kJ/kg, 9,400 kJ/kg, 9,600 kJ/kg, 9,800 kJ/kg, 10,000 kJ/kg, 10,200 kJ/kg, 10,400 kJ/kg, 10,600 kJ/kg, 10,800 kJ/kg, 11,000 kJ/kg, 11,200 kJ/kg, 11,400 kJ/kg, 11,600 kJ/kg, 11,800 kJ/kg, 12,000 kJ/kg, 12,200 kJ/kg, 12,400 kJ/kg, 12,600 kJ/kg, 12,800 kJ/kg, 13,000 kJ/kg, 13,200 kJ/kg, 13,400 kJ/kg, 13,600 kJ/kg, 13,800 kJ/kg, 14,000 kJ/kg, 14,200 kJ/kg, 14,400 kJ/kg, 14,600 kJ/kg, 14,800 kJ/kg, or 15,000 kJ/kg, or the mixture can be subjected to a mechanical energy in the range of from at or about a to at or about b, where a is any one of the preceding mechanical energy values and b is any one of the preceding mechanical energy values that is > a, such as from at or about 1,400 kJ/kg to at or about 7,900 kJ/kg, or at or about 1,300 kJ/kg to at or about 14,400 kJ/kg, etc. For example, for 1 kg material (dry weight basis) in 30 liters of acidified aqueous alcohol processed through a lobe pump (APV type, CL/1/021/10) with a pump motor that is 2 kW at 50 Hz that operated at 10 Hz (0.4 kW) for a period of 50 minutes (3000 seconds), the energy imparted to the sample was 0.4 kW x 3000 seconds or 1200 kilojoules (per kg dry matter).

The mechanical energy can be imparted to the mixture by constant recirculation of the mixture for a period of time from a vessel through a heat exchanger and back to the vessel by a pump, such as a rotary lobe pump, a centrifugal pump, a hydro -transport pump or any combination thereof. The pump can be located before the heat exchanger, or after the heat exchanger. The mechanical energy can be imparted to the mixture by constant recirculation of the mixture through a shell and tube heat exchanger and back to the vessel using a rotary lobe pump. Subjecting the mixture, which includes the bio mass composition and the activating solution, which contains water, an alcohol, and an acid, to the mechanical energy, advantageously enhances the functionality of the activated pectin-containing biomass composition.

In the methods provided herein, the mixture can be heated. The mixture can be heated prior to being subject to mechanical energy. The mixture can be subjected to mechanical energy and then heated. The mixture can be subjected to mechanical energy and heated simultaneously. The mixture can be heated to a temperature of at or about 40°C or greater. The mixture can be heated to a temperature in the range of at or about 40°C to at or about 90°C. The mixture can be heated to a temperature of at or about one of 40°C, 45°C, 50°C, 55°C, 60°C, 65°C, 70°C, 75°C, 80°C, 85°C, and 90°C, or mixture can be heated to a temperature in the range of at or about c to at or about d, where c is any one of the preceding temperatures and d is any one of the preceding temperatures that is > c, such as from at or about 45°C to at or about 85°C, or from at or about 60°C to at or about 80°C, etc.

The mixture can be heated for a period of time that is from at or about 0.1 hr to at or about 2 hours. The mixture can be heated for a period of time of at or about one of 0.1 hr, 0.2 hr, 0.25 hr, 0.3 hr, 0.4 hr, 0.5 hr, 0.6 hr, 0.7 hr, 0.75 hr, 0.8 hr, 0.9 hr, 1 hr, 1.1 hr, 1.2 hr, 1.25 hr, 1.3 hr, 1.4 hr, 1.5 hr, 1.6 hr, 1.7 hr, 1.75 hr, 1.8 hr, 1.9 hr, and 1 hr, mixture can be heated for a period of time in the range of at or about e to at or about f, where e is any one of the preceding times and f is any one of the preceding times that is > e, such as from at or about 0.1 hr to at or about 2 hours, or from at or about 0.25 hr to at or about 2.5 hours, etc.

Combinations of pH, time and temperature can be varied by those skilled in the art while not departing from the spirit of this invention. Such persons will appreciate that variations of such parameters may be employed to modify the total output of cellulosic material, such as the activated pectin-containing biomass composition to be produced in accordance with this invention. In accordance with the disclosure of this invention employing acidic exposure of the starting pectin-containing biomass composition to mechanical energy, conditions of time and temperature can modified depending on the starting pectin-containing biomass composition and other parameters (e.g., dry versus fresh starting biomass) to optimize the yield of the activated pectin- containing biomass composition provided herein. After being heated for the targeted amount of time, the method can include a step for cooling the heated mixture. For example, a cooling medium can be connected to the heat exchanger and the mixture can be cooled to room temperature (from at or about 20°C to at or about 25°C).

After being cooled, the method can include a separation step to separate the fluid components from the mixture. The separation step can be performed in one or more steps. The method can include draining, decanting or membrane filtration of the mixture. For example, the mixture can be deposited on a perforated belt or screen to allow the fluid portion of the mixture to drain away. Excess fluid can be removed by application of a pressure, such as by use of a press, such as a hydraulic press, a pneumatic press, a screw press, a Vincent press, or a cone press, or a centrifugal extractor, or any combination thereof, forming a dewatered activated pectin-containing biomass composition.

The process also can include as a step washing the activated pectin-containing biomass composition with an aqueous alcohol solution to adjust the pH to a range from at or about 3.5 to at or about 4.5, such as a pH of at or about 4.0. The alcohol washing removes the acid. The alcohol wash also can include an alkalizing agent that can neutralize the acid. Exemplary alkalizing agents include an alkali metal salt of a carbonate, bicarbonate, or hydroxide, such as potassium carbonate, sodium bicarbonate or sodium hydroxide. The alcohol wash includes at least 40 wt% alcohol to insure that the pectinaceous material remains insoluble and associated with the cellulosic fiber. Any soluble sugars that were part of the plant cell matrix or produced during processing are removed in the alcohol wash. The alcohol wash can include from at or about 40 wt% to at or about 90 wt% alcohol. The alcohol wash can include from at or about 60 wt% to at or about 80 wt% alcohol. Non-limiting examples of alcohols that can be used to wash the drained fiber include isopropyl alcohol, ethanol, methanol, and combinations thereof.

The amount of alcohol present in the alcohol wash can be increased in subsequent washes. For example, a first alcohol wash can include an alcohol content of 45 wt%; a second alcohol wash can include an alcohol content of 55 wt%; and a third alcohol wash can include an alcohol content of 70 wt% or more. Using an alcohol wash with an alcohol content of 70 wt% or more as a final washing step can efficiently dewater the activated pectin-containing biomass composition prior to drying. This can reduce the time and temperature required to achieve a dried product with a targeted moisture content. The presence of the alcohol also can help to minimize or prevent hydrogen-bond formation between fibrils of the cellulosic fibers of the activated pectin-containing biomass composition, thereby minimizing or preventing hornification of the cellulosic fibers upon drying. The process can include a series of successive alcohol washes having higher alcohol concentrations to dehydrate the activated fiber.

The process also can include a drying step to provide an activated pectin- containing biomass composition in dry form. Exemplary drying methods include using mechanical separation techniques to express water from the fibers, solvent exchange to displace residual water, such as by washing with an organic solvent solution, freeze drying, drying with heat, drying with an air flow, and combinations thereof. An advantage of drying using an organic solvent solution to displace the water as opposed to using heat to evaporate the water is that, once a sufficient amount of solvent is added, the activated pectin-containing biomass composition will release the water and the activated pectin- containing biomass composition can be mechanically pressed to remove the solvent. The high level of solvent in the pores of the activated pectin-containing biomass composition can minimize hydrogen bond formation between fibrils from occurring. In addition to dewatering the fiber, the organic solvent solution also can extract colors, flavors, odors, or a combination thereof from the citrus fiber. The organic solvent solution can include an organic solvent that is polar and water-miscible to facilitate removal of the desired components. Examples the organic solvent solution can include C1-C4 alcohols, such as methanol, ethanol, propanol, isopropanol, and butanol and combinations thereof. The organic solvent in the organic solvent solution can be ethanol or isopropanol or a combination thereof.

The organic solvent solution can include water. The concentration of organic solvent in the organic solvent solution can be in the range of from at or about 70 wt% to about 99 wt%. For example, a 75 wt% aqueous ethanol solution can be used as the organic solvent solution. A 70 wt% aqueous isopropanol solution can be used as the organic solvent solution. The organic solvent solution can remove water-soluble components at lower concentrations or organic solvent and oil- soluble components at higher concentrations of organic solvent. Many solvents, such as isopropanol and ethanol, have a lower heat of vaporization than that of water, and therefore require less energy to volatilize than would be needed to volatilize an equivalent mass of water. The organic solvent can be removed and reclaimed for reuse.

Solvent can be removed from the dewatered activated pectin-containing biomass composition mechanically, such as by belt filtration, decanter centrifugation, decanter bowl centrifugation, disk stack centrifugation, filtering centrifugation, filter press, filtration, membrane filtration, hydrocyclone, pressing between flat surfaces or rollers, porous grating, screen separation, screw press, vortex separator, or other device suitable for removing liquids, or any combination thereof. Solvent drying also can be combined with heat or air or heat and air drying.

The activated pectin-containing bio mass composition can be dried using solvent drying, freeze drying, vacuum drying, spray drying, drum drying, flash drying, fluidized bed drying, blowing with heated gas, exposure to radiant heat, or dried using combinations thereof. A drying agent can be included in the drying process to further inhibit cellulosic to cellulosic interactions. Non-limiting examples of drying agents include glucose syrup, corn syrup, sucrose, dextrins, maltodextrins, and combinations thereof.

The process provided herein also can include a comminuting step, such that the resulting dried activated pectin-containing biomass composition is in a particulate form, e.g. a powder. Non-limiting examples of suitable comminuting methods include grinding and milling. The comminuting step can further reduce the particle size of the dried activated pectin-containing biomass composition to provide a product having improved flowability, dispersability, hydration and/or handling properties. The particles can be comminuted to a size of 300 μιη or less. The particles can be comminuted to a size of 250 μιη or less. The particles can be comminuted to a size of 200 μιη or less. The particles can be comminuted to a size of 150 μιη or less. The particles can be comminuted to a size of 125 μιη or less. The particles can be comminuted to a size of 100 μιη or less. The particles can be comminuted to a size of 75 μιη or less. For example, the particles can be comminuted to a desired size by milling. Any type of mill can be used. For example, any one or a combination of a hammer mill, a pin mill, a pinned disc mill, a beater mill, a cross beater mill, an air micronizer, a jet mill, a classifier mill, a ball mill, a rotary impact mill, and a turbo mill can be a used.

C. PROPERTIES OF THE ACTIVATED PECTIN-CONTAINING BIOMASS

COMPOSITION

One of the properties by which the activated pectin-containing biomass composition can be characterized is the coil overlap parameter of the material. The coil overlap parameter can be used to indicate the functionality of the activated pectin- containing biomass composition. The coil overlap parameter is determined by the following formula:

Coil Overlap Parameter = IV_pectin x Pectin Recovery, wherein the IV_pectin is the intrinsic viscosity of the pectin extracted from the activated pectin-containing biomass composition, and the pectin recovery is the amount of pectin extracted from the activated pectin-containing biomass composition divided by the total amount of activated pectin-containing biomass composition. Thus, the unit of coil overlap parameter is dl/g. The intrinsic viscosity and pectin recovery of the pectin each can be measured using any suitable method. The activated pectin-containing biomass composition when using citrus fruits as the starting pectin-containing biomass composition can have a coil overlap parameter of about 2 or greater. The activated pectin-containing biomass composition for citrus fruits can have a coil overlap parameter from at or about 2 to at or about 4.5, or from at or about 2.3 to at or about 4.5, or from at or about 2.5 to at or about 4.5. The activated pectin-containing biomass composition when using a starting pectin biomass material selected from apple, Jerusalem artichoke or beet can have a coil overlap parameter within the range of at or about 0.5 to at or about 2.0. Further the activated pectin-containing biomass composition can have at least about 300 percent greater than that of a coil overlap parameter of the starting pectin-containing biomass material.

The activated pectin-containing biomass composition has been formed by application of mechanical energy that results in fibrillation of at least a portion of the celluloses present in a biomass from a pectin-rich plant product, such as citrus peel, to tease apart the cellulosic fibers into fibrils. The amount of energy used for fibrillation during processing is not so great as to pull the fibrils completely apart from each other to form cellulosic nanofibers. Instead, the fibrils are teased apart so that at least several fibrils are physically separated and form a web-like reticulated structure with adjacent cellulosic fibrils. The in situ produced pectin component at least partially coats or interacts with the cellulosic fibrils or cellulosic fibers or both.

The activated pectin-containing biomass composition can include from at or about 20 wt% to at or about 50 wt% pectin, and from at or about 80 wt% to at or about 50 wt% cellulosic fiber. The pectin can be present in an amount from at or about 30 wt% to at or about 50 wt% by weight of the expanded pectin-containing biomass composition. The pectin can be present in an amount from at or about 40 wt% to at or about 50 wt%. The pectin can be present in an amount at or about 20 wt%, or at or about 25 wt%, or at or about 30 wt%, or at or about 35 wt%, or at or about 40 wt%, at or about 45 wt%, or at or about 50 wt% by weight of the expanded pectin-containing biomass composition, or in a range between any of these recited values, e.g., the expanded pectin-containing biomass composition provided herein can include from about 35 wt% to about 50 wt% pectin.

The activated pectin-containing biomass composition has a neutral flavor, even when produced from citrus peel. The bitter flavor of citrus peel can be attributed to the presence of d-limonene in the peel. D-limonene is soluble in alcohol, and thus, since the process used to produce the activated pectin-containing biomass composition provided herein includes one or more washing treatments with an alcohol, the amount of d- limonene and other alcohol- soluble rind oils is significantly reduced if not completely removed, resulting in a bland, clean-tasting activated pectin-containing biomass composition. In addition, the peel can be subjected to a stripping process in order to remove d-limonene and other flavor and fragrance oils prior to use of the rind in the process to produce the activated pectin-containing biomass composition. Accordingly, the activated pectin-containing biomass composition can be substantially free of d-limonene and other peel oils. The activated pectin-containing biomass composition provided herein also can be subjected to a stripping process to remove any residual organic solvent used in the process.

When extracted, the pectin component of the activated pectin-containing biomass composition product provided herein has properties of a high methoxy pectin (a pectin having a degree of methoxylation of about 50% or higher). For example, the pectin can form gels at pH values below about 3.5 in the presence of sugar levels above about 60%. Hence, the activated pectin-containing biomass composition provided herein is special and different from citrus fiber of the prior art as it is a mixture of pectin and insoluble cellulosic fibers that have been fibrillated. Because the pectin component of the activated pectin-containing biomass composition provided herein can be present in an amount of up to about 50 wt%, the activated pectin-containing biomass composition provided herein works reasonably well, in pectin applications, such as in the formation of gels, even if not expanded prior to use (explained in detail hereinbelow).

The activated pectin-containing biomass composition is a minimally processed material maintaining the natural pectic substances present in citrus peel. This results in a product containing cellulosic fiber that is not only highly functional, but also closer to nature. Since the pectin is retained and not removed, the resulting activated pectin- containing biomass composition is not a by-product of pectin production and fits with the current trends for a clean label in the food industry. Other cellulose fibers described in the art typically are a waste stream from another extraction process, such as the production of pectin. Important components, such as pectin, are removed in such processes, yielding an inferior cellulose material. Drying and recovery of the "waste" cellulose further can negatively impact any functionality that may have been present. In addition, since the processes typically are optimized for extraction of other targeted materials, such as pectin, there can be a large degree of variability in any cellulose recovered from the waste stream.

The cellulose products of the prior art typically require some added co-agent to provide stability and functionality. Such celluloses also typically provide less surface area, and homification of the cellulose may have occurred prior to or during recovery. These prior art cellulose products can be gritty or coarse because of the homification of the cellulose. To overcome some of these disadvantages, the prior art teaches that the cellulose can be oxidized or bleached or subjected to additional processing steps to provide some functionality. Such processes further remove the final product from the native natural state found in the original biomass.

D. COMPOSITIONS CONTAINING ACTIVATED PECTIN-CONTAINING

BIOMASS COMPOSITION

The activated pectin-containing biomass composition can be used as rheology modifier, contributing viscosity, texture, modification of yield point, modification of elastic modulus, and combinations thereof. The activated pectin-containing biomass composition can be used for thickening, suspension, gelation, stabilizing emulsions, enhancing mouthfeel and body, binding, disintegrating, forming films, and producing stable foams. The activated pectin-containing biomass composition can be used in formulations prepared at room temperature, or in formulations prepared at elevated temperatures, such as up to 100°C for aqueous formulations prepared under atmospheric conditions, or at temperatures greater than 100°C for non-aqueous formulations or for aqueous formulations prepared under pressure. The amount of activated pectin-containing biomass composition to be used depends on the given application and the desired benefit to be obtained, and easily can be determined by the ordinarily skilled artisan in view of the teachings herein and what is known in the art. The activated pectin-containing biomass composition can be present in an amount of from at or about 0.01 wt% to at or about 5 wt% based on the weight of the formulation. The activated pectin-containing biomass composition provided herein can be present in a formulation in an amount at or about 0.01%, 0.025%, 0.05%, 0.075%, 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, 1.1%, 1.2%, 1.3%, 1.4%, 1.5%, 1.6%, 1.7%, 1.8%, 1.9%, 2.0%, 2.1%, 2.2%, 2.3%, 2.4%, 2.5%, 2.6%, 2.7%, 2.8%, 2.9%, 3.0%, 3.1%, 3.2%, 3.3%, 3.4%, 3.5%, 3.6%, 3.7%, 3.8%, 3.9%, 4.0%, 4.1%, 4.2%, 4.3%, 4.4%, 4.5%, 4.6%, 4.7%, 4.8%, 4.9%, or 5.0% by weight of the total formulation, or the activated pectin-containing biomass composition provided herein can be present in a formulation in an amount in the range of at or about g to at or about h, where g is any one of the preceding temperatures and h is any one of the preceding temperatures that is > g, such as from at or about 0.03% to at or about 0.3%, or from at or about 0.2% to at or about 0.8%, etc.

The activated pectin-containing biomass composition can be used to replace a portion of or all of gelatins, starches or derivatives thereof like maltodextrin or dextrose, hydrocolloids, fats, sugars, carbohydrates, proteins or any combination thereof in a formulation. The activated pectin-containing biomass composition can be dispersed in a formulation using a low shear mixer, such as a propeller mixer, or using a high shear mixer, such as a Silverson rotor/stator mixer. Examples of formulations in which the activated pectin-containing biomass composition can be used include a yogurt fruit preparation, a salad dressing, a preserve, a jam, a jelly, a low sugar or no-sugar added fruit spread, a fruit pie filling, a fruit concentrate for ice cream manufacturing, an ice cream topping, a fruit leather, a sorbet, a dairy dessert, an ice cream, an ice milk, a non-dairy dessert, a water ice, a pudding, a custard, a mayonnaise, a low- fat or non-fat mayonnaise, a margarine, a low- fat spread, a sour cream, a low fat or non-fat sour cream, a peanut butter, a nut spread, a chocolate spread, an extruded snack, a soup, a sauce, a gravy, a marinade, a carbonated beverage, an energy drink, a fruit juice, a vegetable juice, a cocoa-based beverage, a chocolate syrup, a dairy beverage, a chocolate milk, a beverage concentrate, an acidified protein drink, a drinkable yogurt, a yogurt, a whipped yogurt, a cheese spread, a processed cheese, a batter, a coating, a whipped topping, a liquid fond concentrate, a bouillon, a whipped topping, a marshmallow product, a confection product, a whipped confection product, a candy, a toothpaste, a dental rinse, a ketchup, a barbeque sauce, a dysphagia product, a breakfast cereal, a baked good, a pastry, a cake, a patisserie, a cookie, a pie crust, a bread, a cracker, a thermostable filling having a low or ultra-low water activity, a dairy product, a meat additive, a meat extender, a paper, a paper coating, a nonwoven, a specialty laid sheet, a dielectric sheet, a battery separator, a capacitor separator, a fracturing fluid, a drilling mud, a weighted or inhibited fluid for oilfield applications, a gravel packing composition, a cementing formulation, a spacer fluid, a pore former in a ceramic or catalyst composition, a flocculation medium, a fining agent, a filter medium, a tub or tile cleaner, a hard surface cleaner, a dish detergent, a floor cleaner, a carpet cleaner, a sanitizer, a wood and furniture polish, a toilet bowl cleaner, an antifog agent, a drain cleaner, a scale remover, a paint, a paint remover, a stain, a stain remover, a dye, a printing ink, a nutraceutical, a pharmaceutical elixir, a suspension, a syrup, a tablet binder, a tablet disintegrant, a pet product, an animal feed product, a shampoo, a conditioner, a cream, a styling gel, a sun screen, a hand or body lotion, a fabric detergent, a high surfactant laundry detergent, a fabric conditioner, a wax suspension, a weed control composition, or an agricultural emulsion.

E. PREPARATION OF EXPANDED PECTIN-CONTAINING BIOMASS

COMPOSITION

The activated pectin-containing biomass composition can be expanded by exposure to extensional stress to form an expanded pectin-containing biomass composition that has a high internal surface area and exhibits unique rheological properties. For example, the expanded pectin-containing biomass composition provided herein can exhibit both time dependent flow (thixotropy) and rate dependent flow (pseudoplasticity). The viscosity of compositions containing the expanded pectin-containing biomass composition is mostly attributable to interactions between the solid particles (e.g., fibrils) of the expanded pectin- containing biomass composition. The texture provided by the expanded pectin-containing biomass composition provided herein is much shorter, being more like a starch than a hydrocolloid gum.

Expansion of the activated pectin-containing biomass composition of the Staunstrup Applications to form the expanded pectin-containing biomass composition provided herein requires application of an extensional stress, to disperse the cellulosic particles and expand the cellulosic fibril network. Little expansion is developed using propeller mixing because it exerts little extensional stress, but expansion occurs. The extensional stress can be achieved by application of high shear, particularly high stress that results in the production of turbulent flow. After expansion by exposure to an extensional stress, viscosity, elastic modulus and yield stress of the expanded pectin- containing biomass composition increase because the cellulose materials present in the activated pectin-containing biomass composition becomes very well dispersed. The extensional stress applied during expansion can be a uniaxial extensional stress.

Exposure to an extensional stress allows the cellulosic fibers activated pectin- containing biomass composition to increase their exposed surface area. The expanding does not have to be optimal to achieve maximum surface area of the cellulosic fiber for the expanded pectin-containing biomass composition to modify rheological or textural properties to a formulation or composition to which it is added. Any expanding of the activated pectin-containing biomass composition by exposure to an extensional stress can increase the exposed surface area of the cellulosic fibers and increase the efficiency of the expanded pectin-containing biomass composition to modify a rheological or textural property.

The extensional stress can be applied to the mixture using any device that can produce turbulent flow. Examples of such devices include propeller mixers, rotor stator mixing devices, such as a Silverson mixer, a toothed-ring disperser, an annular-gap mill or a colloid mill, and homogenizers, such as a pressure or a high pressure homogenizer, a microfluidizer, a French press homogenizer, a counter flow homogenizer and an extensional homogenizer, or any combination thereof. A propeller mixer exerts less extensional stress than a rotor stator mixer, and a rotor stator mixer exerts less extensional stress than a homogenizer.

The extensional stress can be applied using a homogenization treatment. The homogenization treatment can be a pressure homogenization treatment using a pressure homogenizer. Pressure homogenizers can include a piston-type pump or reciprocating plunger in combination with a homogenizing valve assembly affixed to the discharge end of the homogenizer. The homogenization treatment can be a high pressure homogenization treatment using a high pressure homogenizer. Exemplary high pressure homogenizers include the homogenizers of the Gaulin and Rannie series manufactured by APV Corporation (Everett, MA), the Microfluidizer^® homogenizer manufactured by Microfluidics Corp. (Westwood, MA), the HPH homogenizer manufactured by IKA Works, Inc. (Wilmington, NC), and the high pressure homogenizers manufactured by GEA Niro Soavi (Parma, Italy).

Pressure homogenization can expose the activated pectin-containing biomass composition to extensional stress produced by cavitation and turbulent flow. The activated pectin-containing biomass composition can be expanded to produce the expanded pectin-containing biomass composition via one or more passes through a pressure homogenizer depending on the application and desired result. Full expansion can be achieved after 1 pass through a homogenizer at high pressure, or after 2 passes at a lower pressure. The expanded pectin-containing biomass composition can be passed through a high pressure homogenizer a plurality of times, such as at least 2 passes, or at least 3 passes. The pressures used in the pressure homogenization process to activate the activated pectin-containing biomass composition provided herein to yield the expanded pectin-containing biomass composition can be in the range from at or about 1 ,450 to at or about 25,000 pounds per square inch (psi), or from at or about 3,000 to at or about 17,500 psi, or from at or about 4,000 to at or about 14,000 psi, or from at or about 5,000 to at or about 10,000 psi, or from at or about 1,000 to at or about 5,000 psi.

Several parallel homogenization paths can be used for homogenization rather than one large diameter path. A plurality of homogenizers can be used, in series or in parallel or both, to activate the activated pectin-containing biomass composition. In multiple homogenization steps or using multiple homogenizers, the pressure used in each homogenizer or each homogenization step can be the same or different. For example, the first pass can be at a pressure higher than a second pass, such as an initial pressure of at or about 3,500 psi to at or about 10,000 psi, followed by a pressure of at or about 1,000 psi to at or about 3,000 psi. The first pass can be at a pressure lower than a second pass, such as a first pass at a pressure of at or about 1,000 psi to at or about 3,000 psi followed by a second pass at a pressure of at or about 3,500 psi to at or about 9,000 psi. The activated pectin-containing biomass composition provided herein also can be expanded via colloidal milling, high shear blending, extruding, and combinations thereof.

The resulting expanded pectin-containing biomass composition provided herein is functional due to the high surface area of the reticulated cellulosic fiber achieved during exposure to an extensional stress. Unlike water soluble polymers that hydrate so that the molecules are relatively independent of one another, the cellulosic fibers of the expanded pectin-containing biomass composition thicken via formation of a reticulated network of cellulosic fibrils having a very high surface area.

The expanded pectin-containing biomass composition produces a network of insoluble fibers or particles that can interact and "hold" water, creating macroscopic rheological properties. The cellulosic network of the expanded pectin-containing biomass composition contains many pores, throughout which the continuous phase is distributed. On a small scale, such as at 100 μιη or less, the continuous phase viscosity within the pores remains unchanged, with the rheological properties mainly being contributed by the reticulated network and its control of the free movement of the continuous phase. Manipulation of the fiber matrix, such as by increasing or decreasing pore size by using less or more expanded pectin-containing biomass composition allows the end user to adjust the final rheological properties of the composition containing the expanded pectin- containing biomass composition. In addition, controlling the rheological properties of the continuous phase in combination with the network formed by the expanded pectin- containing biomass composition can allow for the selection of different rheological properties of the final product and effective stabilization. Applying less extensional stress during preparation can be compensated for by an increase in use level of the activated pectin-containing biomass composition. However, the rheological properties may change in some respects.

The activated pectin-containing biomass composition can be expanded by exposure of a concentration containing the activated pectin-containing biomass composition at room temperature to an extensional stress, or the concentration can be heated to an elevated temperature, such as up to 80°C for aqueous formulations prepared under atmospheric conditions, or at temperatures greater than 100°C for non-aqueous formulations, and then subjected to an extensional stress, such as high pressure homogenization.

The activated pectin-containing biomass composition can be dispersed in a formulation, such as a salad dressing formulation, and expanded with the other ingredients when the formulation is high shear mixed and/or homogenized to form the expanded pectin-containing biomass composition in situ. The activated pectin-containing biomass composition can be expanded to form a concentrated expanded pectin-containing biomass composition concentration, the concentration of the expanded pectin-containing biomass composition then can be added to the formulation, and mixed with the other ingredients to yield the final product. After dilution, a mild re-expansion can be required to provide full functionality. Without wishing to be bound by any theory, it is postulated that the additional exposure to an extensional stress, such as to a homogenization step, extends the diluted reticulated cellulosic fiber network to incorporate the additional ingredients within its matrix and to fully expand the diluted matrix. Thus, the activated pectin-containing biomass composition can be expanded to form a concentration of the concentrated expanded pectin-containing biomass composition, the concentration of the expanded pectin-containing biomass composition can be added to the formulation, and homogenized with the other ingredients to yield the final product.

Once the activated pectin-containing biomass composition has been expanded to form an expanded pectin-containing biomass composition, the pectin associated with the cellulosic material of the expanded pectin-containing biomass composition can act as a natural co-agent that can minimize or prevent re-aggregation of the expanded cellulosic fiber network. Formation of hydrogen bonds during aggregation of cellulosic fibers can minimize surface area and significantly reduce the efficiency of the reticulated cellulosic fiber product. The pectin co-agent can help minimize hydrogen bond formation between cellulosic fibers. A co-agent can adsorb onto the cellulosic fiber and either by steric bulk or electrical charge can act to inhibit self-association of the cellulosic fibers.

Additional co-agents can be incorporated into a product that is to be thickened using the expanded pectin-containing biomass composition to augment the activity of the pectin already present in the activated pectin-containing biomass composition. The co- agent can be selected to associate with the cellulosic fiber component of the activated pectin-containing biomass composition, and can have a backbone structure that has an affinity for celluloses. The co-agent also can have functional groups that are bulky or charged or both. The co-agent can have a fairly high molecular weight. An exemplary co- agent that can be added to a formulation is a carboxymethyl cellulose (CMC). The carboxymethyl group can provide a charge that reduces the tendency to form cellulose to cellulose associations in the expanded pectin-containing biomass composition. The co- agent can be a medium to high molecular weight CMC with a degree of substitution (DS) of from at or about 0.5 to at or about 0.95. The co-agent can be a CMC with a degree of substitution (DS) of from at or about 0.6 to at or about 0.90 and a molecular weight greater than 100,000 Da. The carboxymethyl cellulose can have a low degree of CM substitution. For example, the carboxymethyl cellulose can have a degree of substitution of at or about 0.2 or less. When additional co-agent is included in a formulation with the expanded pectin-containing biomass composition, it can be present in an amount in the range of from at or about 10: 1 to at or about 2: 1 cellulose:co-agent. Flocculation can occur when the co-agent fails. Flocculation occurs when the cellulosic fibers of the expanded pectin- containing biomass composition self-associate leading to inhomogeneity.

The hydrogen bonding between cellulosic fibers in an expanded pectin-containing biomass composition also can be inhibited by chemical modification of the cellulosic fiber. For example, a fiber surface of the cellulosic fiber of the activated pectin-containing biomass composition can be modified via oxidation or by mild carboxymethyl substitution to inhibit aggregation of the cellulosic fibers in the reticulated network after expansion. F. PROPERTIES OF THE EXPANDED PECTIN-CONTAINING BIOMASS

COMPOSITION

The expanded pectin-containing biomass composition can include from at or about 20 wt% to at or about 50 wt% pectin, and from at or about 80 wt% to at or about 50 wt% cellulosic fiber. The pectin can be present in an amount from at or about 30 wt% to at or about 50 wt% by weight of the expanded pectin-containing biomass composition. The pectin can be present in an amount from at or about 40 wt% to at or about 50 wt%. The pectin can be present in an amount at or about 20 wt%, or at or about 25 wt%, or at or about 30 wt%, or at or about 35 wt%, or at or about 40 wt%, at or about 45 wt%, or at or about 50 wt% by weight of the expanded pectin-containing biomass composition, or in a range between any of these recited values, e.g., the expanded pectin-containing biomass composition provided herein can include from about 35 wt% to about 50 wt% pectin.

The pectin component can be associated with the cellulosic fiber component in such a way that the cellulosic fiber component does not collapse after expansion. Thus, the intrinsic pectin component, formed in situ from protopectin during the production process, can act as a naturally occurring co-agent to prevent or minimize the tendency of cellulosic fibrils to associate, such as due to hydrogen bonding, after expansion. A portion of the pectin component also can be readily dissolved upon expansion, freely diffusing through the continuous phase. When extracted, the obtained pectin has the properties of a HM pectin product. Accordingly, the expanded pectin-containing biomass composition can be viewed as a hybrid between a water soluble polymer and a networked cellulose thickener, capable of exhibiting properties of both, as well as improved or enhanced properties.

The expanded pectin-containing biomass composition can have neutral flavor, even when produced from citrus peel. The expanded pectin-containing biomass composition can be substantially free of d-limonene and other peel oils.

The expanded pectin-containing biomass composition is a minimally processed material maintaining its natural pectic substances in which the high methoxy content contributes to functionality. Since the pectin is retained and not removed, the resulting expanded pectin-containing biomass composition is not a by-product of pectin production and fits with the currents trends for a clean label in the food industry.

The intrinsic viscosity of the expanded pectin-containing biomass composition comes predominately from the pectin component of the activated pectin-containing biomass composition. This water-soluble polymer is hydrated when exposed to water, the hydrated polymer chains acting independently to create a given hydrodynamic volume, forming theoretical spheres that can overlap or interact or both for short or long periods of time, and thus exhibit an intrinsic viscosity. When the activated pectin-containing biomass composition is expanded, the cellulose matrix of the expanded pectin-containing biomass composition influences the rheological properties of the composition in which the expanded pectin-containing biomass composition is present. The viscosity from the reticulated cellulosic network and the contribution from the pectin of the expanded pectin- containing biomass composition arises from the resistance of the reticulated network to laminar shear. The viscosity can drop with continued shear at a constant rate. Due to the strong reticulated cellulosic network in the expanded pectin-containing biomass composition, some stress may have to be applied to begin flow or movement of a formulation containing the expanded pectin-containing biomass composition. The dispersed expanded pectin-containing biomass composition can form a reticulated network full of pores having an effective pore size through which other components of the formulation can move depending on their size. This reticulated network provides physical strength and can physically entrap materials within the pores of the reticulated network. Materials of the formulation that are too large can break the network and cause instability. Particles of the formulation that are too small can pass between and amongst the pores of the reticulated network and are not controlled by the network.

A formulation containing the expanded pectin-containing biomass composition can exhibit a time dependent decrease in viscosity (thixotropy) as the reticulated network breaks upon exposure to shear, and the viscosity of the formulation can return more slowly than exhibited in a formulation thickened with a hydrocolloid polymer solution. Formulations containing the expanded pectin-containing biomass composition also can exhibit pseudoplasticity.

The expanded pectin-containing biomass composition provided herein surprisingly was found to exhibit a synergistic interaction with proteins. It is the reticulated cellulosic network of the expanded pectin-containing biomass composition that provides most of the observed viscosity in systems containing the expanded pectin-containing biomass composition. The pectin component of the expanded pectin-containing biomass composition contributes rheology modification and viscosity. When soluble proteins are present, they can associate to some degree with the reticulated cellulosic network of the expanded pectin-containing biomass composition, or they can be freely diffusing in the continuous phase through the pores of the reticulated cellulosic network or can become entrapped within the pores of the reticulated cellulosic network, such as due to aggregation, or any combination of these states. In the case of a non-interacting system, the protein component, which typically has a low viscosity and has a small impact on overall rheology, can freely diffuse through the reticulated cellulosic network, migrating throughout the pores of the network. In these formulations, any pectin present in the soluble or bound form would contribute little to the viscosity to the formulation and the combination of protein and cellulosic fiber would show a viscosity similar to the cellulose alone.

It has surprisingly been found that the inclusion of certain proteins, or proteins under certain conditions, exhibit an increase in viscosity that is much greater than the addition of the contributions to viscosity of the reticulated cellulosic network and the protein alone. Without wishing to be bound by theory, the synergistic increase in viscosity can indicate that the protein is strongly interacting with the reticulated cellulosic network, or forming particles within the reticulated cellulosic network, or forming its own matrix within the reticulated cellulosic network.

In formulations containing the expanded pectin-containing biomass composition, a synergistic increase in viscosity was observed for soy protein, egg white, sodium caseinate, whey protein and whole milk. The addition of soy protein at its native pH enhances the reticulated cellulosic network of the expanded pectin-containing biomass composition, resulting in a stronger reticulated cellulosic network and exhibits a significant increase in apparent viscosity. This reinforcement remains even when the formulation is heated. Addition of egg white also enhances the reticulated cellulosic network of the expanded pectin-containing biomass composition at neutral pH but shows less interaction when the pH is lowered. Sodium caseinate also enhances the viscosity of systems containing expanded pectin-containing biomass composition. When heated, the caseinate proteins can be denatured and are not as effective in enhancing viscosity. Dropping the pH to 3.8 without heating results in roughly a 40% boost in viscosity of the combined system. Whey protein at an unadjusted pH is more soluble than casein and an enhancement of viscosity of the systems containing expanded pectin-containing biomass composition and whey protein was observed. This holds even after heating if the pH is not adjusted. With an unadjusted pH, a synergistic increase in viscosity was observed in systems containing expanded pectin-containing biomass composition and whole milk. The enhancement of the system viscosity decreased some with heating.

The expanded pectin-containing biomass composition provided herein surprising was found to exhibit a synergistic interaction with hydrocolloids. Without being bound by theory, it is possible that when one or more than one hydrocolloid is present, especially when present during exposure of the activated pectin-containing biomass composition to an extensional stress, the hydrocolloid can associate to some degree with the reticulated cellulosic network of the expanded pectin-containing biomass composition. This association can reinforce the network and make it more resistant to movement. Hence, a reinforced network could exhibit a higher shear viscosity. The hydrocolloid also can be forming its own matrix within the reticulated cellulosic network.

In formulations containing the expanded pectin-containing biomass composition, a synergistic increase in viscosity was observed for starch, xanthan gum and pectin. The addition of starch significantly increased the viscosity. This could suggest that starch can interact strongly with the reticulated cellulosic network. Addition of uncooked starch did not demonstrate the same degree of synergy, and in some instances the uncooked starch granules either provided no enhancement of viscosity, or resulted in a reduction in viscosity. A synergistic increase in viscosity also was observed for xanthan gum and pectin. The synergy, however, was moderate in comparison to the synergy observed with starch.

Several aspects of the activated pectin-containing biomass composition, methods for manufacture thereof, compositions containing the activated pectin-containing biomass composition, methods of activating the activated pectin-containing biomass composition, and the expanded pectin-containing biomass composition and compositions containing the expanded pectin-containing biomass composition are described herein. Features of the subject matter are described such that a combination of different features can be envisioned. For each and every feature disclosed herein, all combinations that do not detrimentally affect the designs, compositions, processes, or methods described herein are contemplated and can be interchanged, with or without explicit description of the particular combination. Accordingly, unless explicitly recited otherwise, any feature disclosed herein can be combined to describe inventive designs, compositions, processes, or methods consistent with the present disclosure.

The activated pectin-containing biomass composition and expanded pectin- containing biomass composition obtained by the process according to the present invention exhibit improved properties over citrus fibers described in the prior art. Electron photomicrographs of the expanded pectin-containing biomass composition and two prior art citrus fibers are shown in FIGS. 1A to 1C. All samples were subjected to the same expansion conditions.

The expanded pectin-containing biomass composition is shown in FIG. 1A. The expanded pectin-containing biomass composition exhibits a reticulated, complex net-like structure. The reticulated network means that movement in one part of the network is coupled to a more distant part of the network via the dispersed interconnected fibrils. The load or stress applied thus can be effectively spread over a larger area. This configuration of the reticulated cellulosic network results in the highest rheological properties, including elastic modulus, yield stress and a thixotropic steady shear flow. The prior art citrus fiber products do not exhibit this extent of reticulated cellulosic network.

The Fibergel LC (Florida Food Products, Eustis, FL) citrus fiber is shown in FIG.

IB. The cellulose fibers are not fibrillated into smaller diameter fibrils, and there is no fine mesh network present. The Ceamsa Ceamfibre citrus fiber is shown in FIG. 1C. As can be seen, while the cellulose fibers show some fibrillation, the fibrils are associated with the cellulose fibers and do not form a reticulated network. Fibrils with distinct ends are visible. Such fibrils act more independently than a reticulated network, and when an external force is applied, each fibril will be free to move to that force independently. In such situations, viscosity will be lower and there may be little observable elastic modulus and yield stress in compositions containing such fiber until the fiber content is about 1%.

An aqueous concentration of an expanded pectin-containing biomass composition can be prepared and used. The expansion step can include preparing an aqueous concentration of the activated pectin-containing biomass composition and passing the concentration through a homogenizer. The homogenizer can be a high pressure homogenizer, a French press, a microfluidizer, or any combination thereof. The concentration of the expanded pectin-containing biomass composition concentration can include a preservative if the suspension is to be stored for an extended period of time. Exemplary preservatives include ascorbic acid, citric acid, sorbic acid, benzoic acid, propionic acid and metal salts thereof, chlorhexidine di-gluconate, benzyl alcohol, benzalkonium chloride, parabens, natamycin, and/or combinations thereof.

G. COMPOSITIONS CONTAINING EXPANDED PECTIN-CONTAINING

BIOMASS COMPOSITION

The expanded pectin-containing biomass composition provided herein can provide thickening, texture, rheological properties or processability or stability to a large number of products used in the food, beverage, snack, industrial, oilfield, paint, paper, pharmaceutical, nutraceutical, personal care, household care and cosmetics industries. The expanded pectin-containing biomass composition is an excellent emulsion stabilizer and demonstrates very good activity as a texture building agent. The amount of expanded pectin-containing biomass composition to be used depends on the given application and the desired benefit to be obtained, and easily can be determined by the ordinarily skilled artisan in view of the teachings herein and what is known in the art. The expanded pectin- containing biomass composition provided herein can be used in any application where a hydrocolloid such as starch or xanthan gum is useful.

As discussed below, the expanded pectin-containing biomass composition provided herein is a functional ingredient that can be used in various food applications. For example, the expanded pectin-containing biomass composition can be used as a gel former, such as in jams and jellies; as a texture enhancer, such as in beverages and ice creams; as a partial flour replacement in baked goods such as breads or cakes; as a stabilizer for salad dressings and mayonnaise; in the extrusion of cereals and extruded snack foods; as a suspension aid in beverages; as a thickening agent in puddings and desserts; as a foam stabilizer in whipped cream and ice cream, and in protein stabilized foams such as meringue and marshmallows; and to provide storage stability.

The expanded pectin-containing biomass composition provided herein can be added to a formulation in an amount to provide identifiable benefits, and can be as low as 0.001 wt%, and can be included in amounts of 2 wt% or higher, such as in some film- forming tableting applications. The expanded pectin-containing biomass composition provided herein can be added to a formulation in an amount from at or about 0.001% to at or about 2% by weight of the total formulation, or in an amount from at or about 0.005% to about 1.5% by weight of the total formulation, or in an amount from at or about 0.005% to about 1.0% by weight of the total formulation, or in an amount from at or about 0.01% to about 0.75% by weight of the total formulation, or in an amount from at or about 0.1% to about 0.5% by weight of the total formulation. In some film-forming applications, the expanded pectin-containing biomass composition can be present at levels greater than at or about 1% by weight of the total formulation. Persons of ordinary skill in the art will appreciate that varying amounts of the expanded pectin-containing biomass composition will be appropriate for different functional uses. The expanded pectin-containing biomass composition provided herein can be present in a formulation in an amount at or about 0.001%, 0.0025%, 0.005%, 0.0075%, 0.01%, 0.02%, 0.03%, 0.04%, 0.05%, 0.06%, 0.07%, 0.08%, 0.09%, 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, 1.1%), 1.2%), 1.3%), 1.4%), 1.5%) or 2%> by weight of the total formulation, or the expanded pectin-containing biomass composition provided herein can be present in a formulation in an amount in the range of at or about i to at or about j, where i is any one of the preceding temperatures and j is any one of the preceding temperatures that is > i, such as from at or about 0.03% to at or about 0.3%, or from at or about 0.2% to at or about 0.8%, etc. Because of its inherent pectin content of from at or about 20 wt% to at or about 50 wt% pectin (measured on a dry basis), the expanded pectin-containing biomass composition provided herein can be used in applications in which pectin traditionally is used. Such applications can include acidified protein drinks, stirred yoghurt, fruit drinks, preserves, jams and jellies, low sugar jams and jellies, low sugar fruit spreads, yogurt fruit preparations, fruit leathers, fruit pie fillings, confection products, fruit concentrates for ice cream manufacture, and ice cream toppings.

The expanded pectin-containing biomass composition provided herein can be used to modify the rheology, texture or processability of many food products. For example, the expanded pectin-containing biomass composition can be used to partially or completely replace fats and oils in some formulations to produce low fat or non-fat formulations. For example, the oil in salad dressings, mayonnaise, whipped toppings, spreads, sour cream, yogurt, dairy products, ice cream, sauces, gravies, soups, peanut butter, nut spreads, chocolate spreads, cheese spreads, process cheese, reduced fat spreads, and meat additives or extenders can be partially or fully replaced with from at or about 0.01 wt% to at or about 2 wt% expanded pectin-containing biomass composition provided herein based on the total weight of the formulation. The expanded pectin-containing biomass composition provided herein demonstrates remarkable emulsion stabilizing properties.

The expanded pectin-containing biomass composition provided herein can be used to provide emulsion stability in full fat salad dressing, to replace a portion or all of the fat in salad dressings and mayonnaise, and to replace a portion or all of the stabilizers, starch, maltodextrin and egg yolk. Formulations containing the expanded pectin-containing biomass composition provided herein also exhibit good cling properties, and the higher yield stress produced by the presence of the expanded pectin-containing biomass composition results in a product that demonstrates good flow properties. The presence of the expanded pectin-containing biomass composition can result in a product having a mouthfeel similar to a full fat formulation even when a large portion or all of the oil or fat component has been replaced. The expanded pectin-containing biomass composition can be used alone or in combination with hydrocolloid thickeners, such as starch or xanthan gum, to attain the desired flow and cling properties. The amount of expanded pectin- containing biomass composition that can be present in the formulation can be from at or about 0.01 wt% to at or about 2 wt% based on the total weight of the formulation.

The expanded pectin-containing biomass composition can be used to fully or partially replace starch in some formulations to produce a lower calorie formulation. For example, all starch can be replaced in dressings, and mayonnaise or a portion of the starch or flour in soups, gravies, sauces, batters, cakes, biscuits, dough, crusts, and puddings can be replaced with from at or about 0.001 wt% to at or about 2 wt% expanded pectin- containing biomass composition provided herein based on the total weight of the formulation, while maintaining the functional properties of the product. The characteristic bite and texture of puddings can be maintained by including the expanded pectin- containing biomass composition to provide a range of yield values in the final product. The reduced calorie product containing the expanded pectin-containing biomass composition can maintain commercially acceptable physical and processing characteristics.

The expanded pectin-containing biomass composition can be used to partially or completely replace eggs in food formulations. For example, egg yolks or egg whites in ice cream, meringues, baked goods, dressings and sauces, can be fully or partially replaced with the expanded pectin-containing biomass composition provided herein. Exemplary baked goods include bagels, biscuits, breads, brownies, buns, cookies, cakes, crackers, doughnuts, muffins, pastries, patisserie, pie crusts, pita breads, pizza crusts, tarts, tortes, and waffles. The expanded pectin-containing biomass composition provided herein demonstrates texture building and stabilizing properties in such formulations. The amount of expanded pectin-containing biomass composition that can be present in the formulation can be from at or about 0.01 wt% to at or about 2 wt% based on the total weight of the formulation.

The expanded pectin-containing biomass composition can provide a pleasant mouthfeel or texture to beverages, jams, and juices, and to suspend pulp components when present or bring back mouthfeel in fruit beverages where all or part of pulp/pure has been replaced. Exemplary beverages include fruit flavored drinks, fruit juices, fruit juice concentrates, flavor concentrates (in liquid form) for carbonated beverages, energy drinks, cocoa-based drinks (such as cold chocolate flavored drinks or chocolate milk, or hot beverages such as hot chocolate), dairy beverages, buttermilk, drinkable yogurts, plant- based milks (such as almond, cashew, coconut, hazelnut or soy milks), and vegetable juices. The beverage can include suspended pulp or other particles, such as tapioca pearls, chewy cubes from young coconut, and nata de coco jellies or particles. The expanded pectin-containing biomass composition can suspend these particles and allow formulations of visually unique products. The expanded pectin-containing biomass composition also can suspend cocoa powder or particles, such as in chocolate syrups, chocolate milk, and chocolate beverages. The expanded pectin-containing biomass composition also can suspend plant particles, such as tomato pulp in ketchup and barbeque sauce, or spices, such as ground mustard in mustard preparations or fruit pieces in yoghurt fruit preparations. The amount of expanded pectin-containing biomass composition that can be present in a formulation can be from at or about 0.005 wt% to at or about 2 wt% based on the total weight of the formulation.

The expanded pectin-containing biomass composition can be used to stabilize compositions that include air-in-liquid dispersions, such as ice cream, froths and foams, whipped toppings and marshmallows. Air bubbles can become entrapped within the reticulated cellulosic network of the expanded pectin-containing biomass composition and are stabilized by the reticulated network, which can prevent or minimize their migration or coalescence into larger air bubbles. The stabilized air bubbles can result in stabilized aerated products. Inclusion of the expanded pectin-containing biomass composition in aerated product formulations also can result in products that exhibit higher yield values. The pectin associated with the cellulosic fibers of the reticulated cellulosic network of the expanded pectin-containing biomass composition also can help to maintain liquid around the air bubbles, further helping to stabilize the aerated product or the ice cream during storage.

Accordingly, the expanded pectin-containing biomass composition can be used in aerated products such as whipped creams, whipped cream substitutes, ice creams to improve overrun and stabilize, confectionary coatings or fillings, whipped yogurts, whipped chocolates or caramels, marshmallow products, and meringues. The air can be injected or incorporated into the composition to form air bubbles within the composition, such as using an apparatus or method described in U.S. Pat. Nos. 5,000,974 (Albersmann, 1991); 5,433,967 (Kateman et al, 1995); and 6,951,660 (Brown et al, 2005). The expanded pectin-containing biomass composition also can be used in whipped cosmetic and pharmaceutical formulations, and to entrain air in some industrial products. The amount of expanded pectin-containing biomass composition present in the formulation can be in an amount of from at or about 0.001 wt% to at or about 2 wt% based on the total weight of the formulation.

The expanded pectin-containing biomass composition provided herein can be used for fat mimicry, rheology modification and stabilizing foam of frozen dairy products. The texture of frozen dairy products can be modified by the incorporation of air during the freezing process (overrun). Replacing the existing stabilizer blend or including the expanded pectin-containing biomass composition can result in a frozen dairy product, such as an ice cream, ice milk, dairy dessert (e.g., frozen custard or soft serve ice cream), water ice or sorbet having a light texture and smooth mouthfeel. The expanded pectin-containing biomass composition provided herein also can be used to thicken dairy products, such as milk shakes, custards, yogurts and the base for ice cream while allowing removal of some or all of the fat while maintaining the texture and mouthfeel of the full fat versions of the products. These properties can be attained at use levels of the expanded pectin-containing biomass composition significantly lower than the amount of locust bean gum or guar gum to achieve the same viscosities. The low use level of the expanded pectin-containing biomass composition provided herein can result in significant cost savings while providing a product that exhibits high quality taste and rich, creamy texture. The amount of expanded pectin-containing biomass composition that can be present can be from at or about 0.01 wt% to at or about 2 wt% based on the total weight of the formulation.

The ability of the expanded pectin-containing biomass composition provided herein to stabilize emulsions while exhibiting good yield stress makes the expanded pectin- containing biomass composition ideal for use in condiments and low calorie or low fat spreads. These products typically are emulsions with either the fat or the aqueous portion as the continuous phase. The expanded pectin-containing biomass composition can be included to reduce the amount of fat present in the formulation while yielding a stable and spreadable product that exhibits a creamy mouthfeel. The amount of expanded pectin- containing biomass composition that can be present can be from at or about 0.01 wt% to at or about 2 wt% based on the total weight of the formulation.

The expanded pectin-containing biomass composition provided herein also can be used in applications to prevent yield loss in prepared meat products, such as cold cuts, bologna, hot dogs and other emulsified sausages. These meat products are essentially oil- in-water emulsions that contain comminuted meat particles. Emulsifiers can be added to stabilize the emulsion, or the meat proteins by themselves can serve as emulsifiers. Water loss during processing and cooking can result in weight loss or shrinkage of the product. The reticulated cellulosic network of the expanded pectin-containing biomass composition can help stabilize the emulsion during processing, and can provide a more circuitous path thereby minimizing water migration out of the product, minimizing liquid loss thereby minimizing yield loss and product shrinkage during cooking. The amount of expanded pectin-containing biomass composition that can be present can be from at or about 0.01 wt% to at or about 2 wt% based on the total weight of the formulation. The expanded pectin-containing biomass composition can be used in the preparation of a cellulose casing for stuffing with meat products, such as for the production of sausage products. Inclusion of the expanded pectin-containing biomass composition to the traditional material used to form the cellulosic casing can improve the adhesion of the casing to the meat without becoming too strongly associated with the meat so at to prevent removal. Inclusion of the expanded pectin-containing biomass composition in an amount from at or about 0.005 wt% to at or about 0.5 wt% based on the total weight of the casing formulation can result in a casing that promotes adhesion of the casing to the meat, allows shrinkage of the casing with the meat as it is processed, and can exhibit a good release profile from the meat when the casing is to be separated from the meat.

The expanded pectin-containing biomass composition provided herein also can be used in icings and frostings to provide texture and stability while allowing for reduction of the amount of fat or sugar or both in the formulation. The reticulated cellulosic fiber network of the expanded pectin-containing biomass composition also can be used to modify the texture of certain confectionary products, such as fudge, marshmallow, licorice, gummi bears, gum drops, a jelly foam, a nougat, and starch jelly candies. The expanded pectin-containing biomass composition can enhance the bite of the product, and can allow inclusion of particles that normally cannot be suspended in the hot formulation for a period long enough to be distributed in the final confection. The expanded pectin-containing biomass composition provided herein also can be used to provide texture and stability to dysphagia products. The amount of expanded pectin-containing biomass composition that can be present can be from at or about 0.001 wt% to at or about 2 wt% based on the total weight of the formulation.

The expanded pectin-containing biomass composition provided herein can be used as a binder to hold non-animal proteins together to form a meat extender. Texturized vegetable proteins, such as soybean, pea and cottonseed proteins, wheat gluten, mycoprotein (from fungal sources such as mushrooms), and oilseed or cereal proteins, such as albumins, globulins, gliadins, and glutelins can be combined to form a meat substitute or meat extender that provides a well-balanced amino acid profile. The expanded pectin-containing biomass composition can be mixed with the proteins and extruded into a desired shape, such as granules, chunks, or flakes. The expanded pectin- containing biomass composition can help provide a meat-like texture, as well as maintain structural integrity of the resulting product. The amount of expanded pectin-containing biomass composition that can be present can be from at or about 0.01 wt% to at or about 2 wt% based on the total weight of the formulation. To promote film formation, the amount of expanded pectin-containing biomass composition that can be included can be greater than 2 wt%.

The expanded pectin-containing biomass composition provided herein can be used as a binder to hold ingredients or components of a formulation together. For example, some ready-to-eat cereals contain aggregates of flakes, nuts, dried fruits or grains in any combination. The binder typically used to hold these components together can include a high amount of sugar or fat. The expanded pectin-containing biomass composition provided herein can bind the material together without the added calories contributed by fat and sugar, and also provides soluble and insoluble fiber components. As the components are heated to remove water from the applied expanded pectin-containing biomass composition binding the components together, the cellulosic fibers of the reticulated cellulosic network of the expanded pectin-containing biomass composition can strongly associate with the other components, such as via hydrogen bond formation, binding the components together. The expanded pectin-containing biomass composition provided herein also can be used in the preparation of extruded products, such as breads, cereals, doughs and snack foods. The presence of the expanded pectin-containing biomass composition product can hold together components as they pass though the extruder, facilitated by the shear thinning characteristics of the expanded pectin-containing biomass composition. The extruded cereal formulations can be extruded in any shape, such as flakes, shreds, or puffed shapes, including hexagons, rings, rounds, spheres, triangles, and tubes. The expanded pectin-containing biomass composition provided herein also can be used in the preparation of confectionery coatings and/or fillings that can be used with the extruded products. The amount of expanded pectin-containing biomass composition that can be present can be from at or about 0.005 wt% to at or about 2 wt% based on the total weight of the formulation.

The expanded pectin-containing biomass composition provided herein can be used for the production of pet products and animal feed products. For example, the expanded pectin-containing biomass composition provided herein can be used to bind animal protein, meats, meat by-products and grains together to form a pet food product. The pet food can be a moist or dry form, typically formed in one or a plurality of shapes, sizes and colors. The pet food or animal feed product can be in a pelletized kibble form. The kibbles can be formed by an extrusion process in which the ingredients are formed into a dough-like mixture and extruded under heat and pressure to form the pelletized kibble form. The expanded pectin-containing biomass composition can help maintain the dispersion of components in the material as it is processed and extruded. The extrusion technology provides an inexpensive and efficient method for production of animal feed kibbles, and the inclusion of the expanded pectin-containing biomass composition also can increase the strength of the mixture during handling and after extrusion. The amount of expanded pectin-containing biomass composition that can be included can be from at or about 0.005 wt% to at or about 2 wt% based on the total weight of the formulation.

The expanded pectin-containing biomass composition provided herein can be used for the production of moist pet products and animal feed products. These products can contain proteinaceous particles, such as egg or cottage cheese pieces, to increase the nutrition provided thereby and to improve palatability. Some of the added proteinaceous particles are not stable to retort conditions and can structurally degrade. Addition of the expanded pectin-containing biomass composition provided herein to the proteinaceous particles can help to maintain structural integrity during the manufacturing process. The amount of expanded pectin-containing biomass composition that can be included can be from at or about 0.01 wt% to at or about 2 wt% based on the total weight of the formulation.

The expanded pectin-containing biomass composition provided herein can be used for the formation of an edible film. The edible film can be a food product, such as a fruit leather, or a batter or coating, or can be used as an edible packaging material. For example, when included in a batter or coating and the batter or coating is fried, the water is driven out of the batter or coating, resulting in the cellulosic fibers of the expanded pectin- containing biomass composition to form hydrogen bonds, with other components of the formulation or with cellulosic fiber of the network, which can result in formation of a film. The film can allow steam to escape from the inside of the coating while minimizing the entry of the hot oil through the coating, minimizing fat uptake by the food product. When used as an edible packaging material, the formulation can include one or more other edible film- forming material, such as a cellulose derivative, a protein, an alginate, a xanthan gum, gum arabic, or any combination thereof. As water in the formulation is removed, the cellulosic fibers of the expanded pectin-containing biomass composition can form hydrogen bonds with the other components, which can result in a film that exhibits high tensile strength and tear resistance. Depending on the extent of the hydrogen bonds developed during the drying process, the resulting film may not easily rehydrate when exposed to water. The amount of expanded pectin-containing biomass composition that can be present can be from at or about 0.01 wt% to at or about 2 wt% based on the total weight of the formulation.

The expanded pectin-containing biomass composition can be used to reduce the total calorie count of a food product by replacing one or more of a fat, carbohydrate or protein. The expanded pectin-containing biomass composition includes a combination of soluble and insoluble fiber and contributes few calories, significantly less than an equivalent amount of fat. Accordingly, the expanded pectin-containing biomass composition can impart stabilization, structure and improved rheological properties while removing higher calorie components from the formulation. The expanded pectin- containing biomass composition can be used to reduce the overall calorie count of an emulsion, foam, gel, dispersion, or any combination thereof. The reduced calorie product can maintain commercially acceptable physical and processing characteristics. The amount of expanded pectin-containing biomass composition that can be present can be from at or about 0.001 wt% to at or about 2 wt% based on the total weight of the formulation.

The expanded pectin-containing biomass composition can be used to produce edible non-aqueous thermostable compositions contain a chaotropic agent. Exemplary chaotropic agents include corn syrup, a carboxymethyl cellulose, sucrose and combinations thereof. The thermostable compositions can be used to prepare thermostable fillings having low or ultra-low water activity (e.g., at or about 0.5 or less, such as from at or about 0.2 to at or about 0.4). The thermostable fillings containing the expanded pectin- containing biomass composition can be sweet or savory. The thermostable fillings can be extruded or used in laminated products, such as for the filling in sandwich cookies, filled confections having creme centers, and filled bakery products such as pretzels, pastries, and crackers. The amount of expanded pectin-containing biomass composition that can be present can be from at or about 0.005 wt% to at or about 2 wt% based on the total weight of the formulation.

Another benefit that can be attributed to the inclusion of the expanded pectin- containing biomass composition in a food formulation is the improved flavor release characteristics that can be achieved compared to formulations thickened using starch or other hydrocolloids. In the products containing the expanded pectin-containing biomass composition, the essential oils of the flavors can be distributed in the pores of the reticulated cellulosic matrix of the expanded pectin-containing biomass composition, where they are stable. Upon chewing, the essential oils can easily migrate out of the reticulated cellulosic network and be perceived by the taste buds. Since the inclusion of the expanded pectin-containing biomass composition can reduce or eliminate other hydrocoUoids in a formulation, which can coat the tongue and interfere with the perception of the flavor, it can be possible to use reduced amounts of flavorings in a formulation. The amount of expanded pectin-containing biomass composition that can be present can be from at or about 0.001 wt% to at or about 2 wt% based on the total weight of the formulation.

The expanded pectin-containing biomass composition also can be used in non-food applications to modify the rheology or stabilize the components of the formulations. For example, the expanded pectin-containing biomass composition can be dispersed in a polyol fluid, and when expanded can provide a structure effective in exhibiting yield stress. The yield stress achieved imparts excellent stability to such products and the products can be used in a variety of industrial applications. For example, when the expanded pectin-containing biomass composition is used to prepare a thermal insulation fluid, the reticulated cellulosic fiber network of the expanded pectin-containing biomass composition can minimize or prevent the formation and circulation of thermal convection currents. The expanded pectin-containing biomass composition also can be used to prepare fluid carrier or delivery compositions, in which the reticulated cellulosic fiber network of the expanded pectin-containing biomass composition suspends particulate materials, such as sand, clay, and metal cuttings, resulting in stable suspensions of particulates that do not settle out. Accordingly, the expanded pectin-containing biomass composition provided herein is useful for the preparation of metal working fluids, lubricants, fracturing fluids, well bore drilling muds, weighted or inhibited fluids for oilfield applications, workover/completion fluids, gravel packing applications, cementing, spacer fluids, printing inks, dyes, cosmetics, toothpastes, personal care products, nutraceuticals, and pharmaceuticals, such as elixirs, suspensions, and syrups. The amount of expanded pectin-containing biomass composition that can be present can be from at or about 0.01 wt% to at or about 2 wt% based on the total weight of the formulation. For some applications where the continuous phase is non-aqueous or contains high levels of solutes, such as salts, glycerol or polyols, the amount of expanded pectin-containing biomass composition that can present in the formulation can be greater than 2 wt%.

In addition to suspension of particles, polyol compositions Theologically modified by the inclusion of the expanded pectin-containing biomass composition provided herein also can improve cling of the formulations, and can provide anti-sag properties. Accordingly, the expanded pectin-containing biomass composition provided herein can be included in compositions to enhance cling or to provide anti-sag properties or both in such applications as paints, stains, varnishes, paint or varnish removers, tire sealants, and lubricants, inks and dyes, such as to minimize or prevent the compositions from flowing once applied to a surface of an object. The amount of expanded pectin-containing biomass composition that can be present can be from at or about 0.005 wt% to at or about 0.75 wt% based on the total weight of the formulation. For each application, the amount of the expanded pectin-containing biomass composition provided herein is added to yield a rheo logically modified fluid composition comprising a polyol to have a viscosity appropriate for the specific application, and to allow the final formulation to be applied by spraying, pouring, or pumping onto the surface of the object.

The expanded pectin-containing biomass composition provided herein also can be used in the preparation of paper, paper coatings and nonwovens. The tensile strength of wet sheets and dry sheets increases as the concentration of the expanded pectin-containing biomass composition present increases. The pore size of the produced product also can decrease with increasing concentrations of the expanded pectin-containing biomass composition. The expanded pectin-containing biomass composition can be used in conjunction with plant fibers, such as hardwood and softwood fibers, cotton and hemp fibers, and combinations thereof, as well as with non-cellulose fibers, including nylon, rayon, polyester, aramid, modacrylic, acrylics, polyolefm, polypropylene, kevlar and blends thereof, or an inorganic fiber made of glass, carbon, silicon or carbide, or a metal fiber, such as copper or stainless steel, and any combination of these fibers. The expanded pectin-containing biomass composition can perform well in many application areas, and is suitable for use in a broad spectrum of products, including nonwovens for medical and hygiene applications, specialty wet-laid papers, friction material, filter paper and filtration material, such as a microporous cellulose filter. The amount of expanded pectin- containing biomass composition that can be present can be from at or about 0.005 wt% to at or about 2 wt%.

The expanded pectin-containing biomass composition can be used in preparation of a paper coating for improved printing characteristics. The coating can be applied using a machine coater. After applying the coating containing the expanded pectin-containing biomass composition, printing characteristics such as smoothness and gloss can be improved by application of a calendering treatment. The exposure of the coating containing the expanded pectin-containing biomass composition provided herein to the heat and pressure of a calendaring treatment can result in a paper that exhibits improved printing properties compared to a calendared paper that was not coated with the expanded pectin-containing biomass composition. A paper coating containing the expanded pectin- containing biomass composition provided herein, after application to the paper web surface and subjecting the web to a calendaring treatment, can enhance one or more surface properties such as gloss, ink holdout, ink receptivity, smoothness and surface strength. The amount of expanded pectin-containing biomass composition applied as a coating can be in the range of from at or about 1 kg per metric tonne (kg/t) of paper to at or about 10 kg/t. The coating can include an organic pigment, a mineral pigment, a filler, a starch, a polymeric additive, or any combination thereof.

The expanded pectin-containing biomass composition can be used in the production of dielectric sheets or separators for batteries and capacitors. In batteries, these separators are located between the cathode and the anode material and electrically insulates the cathode from the anode material, but which absorbs electrolyte and allows water transport and ion transfer between the electrodes. The battery separator paper can be a nonwoven fabric. The battery separator paper can include plant-based cellulose fibers, alone or in combination with polymeric fibers, such as nylon, vinylon, rayon, vinylon-rayon blend, polyolefm and combinations thereof. The film-forming properties of the reticulated cellulosic fiber of the expanded pectin-containing biomass composition can be used to modify the surface properties of the dielectric sheets or separator sheets, and can modulate the porosity of the final product, while maintaining the ionic permeability of the sheet. The amount of expanded pectin-containing biomass composition that can be present can be from at or about 0.001 wt% to at or about 2 wt% based on the total weight of the sheet.

The expanded pectin-containing biomass composition can be used in the production of porous materials, such as the control of ceramic porosity, the manufacture of catalysts, and in filtration devices. The expanded pectin-containing biomass composition can be incorporated into the raw unfired material, suspending the components of the product in the reticulated cellulosic network of the expanded pectin-containing biomass composition. The expanded pectin-containing biomass composition can provide plasticity and can increase green strength and workability. When fired, the expanded pectin- containing biomass composition burns out, leaving negative space in the fired product, resulting in a network of micro- or nano-sized pores. The amount of expanded pectin- containing biomass composition that can be present in a formulation can be from at or about 0.001 wt% to at or about 2 wt% based on the total weight of the formulation.

The expanded pectin-containing biomass composition provided herein can be used for the preparation of agricultural products, pesticides, crop protection products, and herbicide products. These products can include emulsions in water containing a non-polar dispersed phase in an aqueous continuous phase, suspension concentrates containing solid active ingredients dispersed in liquids, or suspoemulsions containing oil phases as emulsions in water and solid phases dispersed in the water. The expanded pectin- containing biomass composition can suspend the solid active ingredients and prevent their aggregation or precipitation. The expanded pectin-containing biomass composition can suspend the dispersed phase of any emulsion and prevent coalescence of the dispersed particles. The amount of expanded pectin-containing biomass composition present in such compositions can vary depending on the desired viscosity of the composition necessary for a specific use. For example, the expanded pectin-containing biomass composition can be present in an amount from at or about 0.01% to at or about 2% by weight of the total weight of the composition. When diluted to use strength, the material can be applied using a pressure atomizer, having an orifice large enough to allow the expanded pectin- containing biomass composition to pass. The passage through the atomizer under pressure can exert sufficient extensional stress on the diluted product to further extend the cellulosic matrix, providing viscosity, cling and sag resistance to the product in use. Accordingly, the product tends to stay where applied, increasing the efficacy of the material supplied, and can minimize or prevent overspray or drift.

The expanded pectin-containing biomass composition provided herein can be used for the preparation of suspensions, emulsions or foams having an acidic, alkaline or neutral pH and can be formulated to be compatible with cationic materials, such as cationic surfactants, anti-microbials, disinfectants, sanitizers and agricultural ingredients, such as cationic pesticides or herbicides. When dispersed in such formulations, the expanded pectin-containing biomass composition can be expanded to produce a highly viscous, thixotropic mixture that exhibits high yield stress. The amount of expanded pectin-containing biomass composition present in such compositions can vary depending on the desired viscosity of the composition necessary for a specific use. For example, the expanded pectin-containing biomass composition can be present in an amount from at or about 0.1% to at or about 2% by weight of the total weight of the composition. When cationic ingredients are present in the formulation at levels greater than 0.1 wt%, a cationic-compatible co-agent can be included. Exemplary cationic co-agents include cationic hydroxyethyl cellulose, a cationic starch, conventional cationic starch, cationic guar, and chitosan, a cationic surfactant, and combinations thereof. The amount of cationic co-agent that can be included in the compositions can be in the range from at or about 0.05% to at or about 1% by weight of the composition. The amount of cationic co- agent that can be included in the compositions can be greater than 0.1 wt% or less than 0.85 wt%.

The expanded pectin-containing biomass composition provided herein can be used for the preparation of suspensions or emulsions containing surfactants, alone or in combination with fragrances. The expanded pectin-containing biomass composition remains viscous and homogeneous in the presence of surfactants, even at high loading levels of surfactants, such as are present in high efficiency liquid laundry products. The surfactant and/or fragrance can be added prior to, simultaneously with, or subsequent to, the dispersion/expansion of the expanded pectin-containing biomass composition. In some applications, in order to minimize foam generation, surfactant is added after expansion of the expanded pectin-containing biomass composition. The expanded pectin- containing biomass composition is useful in household care products such as cleaners, hard surface cleaning products, abrasive cleaners, foaming cleaners, disinfectants and disinfectant cleaners, drain openers, oven cleaners, toilet bowl cleaners, tub and tile cleaners, upholstery cleaners, carpet and rug cleaners, microwave oven cleaners, wax suspension, and in fabric care products, such as fabric conditioners, liquid fabric detergents and high efficiency liquid laundry detergents. The amount of expanded pectin- containing biomass composition present in such compositions can vary depending on the desired viscosity of the composition necessary for a specific use. For example, the expanded pectin-containing biomass composition can be present in an amount from at or about 0.01% to at or about 2% by weight of the total weight of the composition.

The activated pectin-containing biomass composition provided herein can be used without expansion as a flowability aid, binder, disintegrant and diluent in the manufacture of compressed tablets, such as for pharmaceutical, personal care and household care markets. The dry form of the activated pectin-containing biomass composition provided herein can act as a disintegrant when incorporated into the tablet matrix. The activated pectin-containing biomass composition provided herein also can enhance liquid transport into the tablet matrix, which can accelerate dissolution of the tablet. The amount of expanded pectin-containing biomass composition that can be present as a binder or disintegrant can be from at or about 0.1 wt% to at or about 20 wt% based on the total weight of the formulation.

Because of its compatibility with acidic, alkaline and neutral pH components, as well as stability in the presence of fragrances, oils and surfactants, the expanded pectin- containing biomass composition provided herein can be used for the preparation of suspensions or emulsions for personal care products or cosmetics. Personal care products include cosmetic formulations, hair care products such as shampoos, conditioners, creams, styling gels, personal washing compositions such as body washes, soaps and make-up removers, sun screen creams, hand and body lotions, shaving creams, toothpaste, and hand sanitizers. Inclusion of the expanded pectin-containing biomass composition can allow suspension of larger particles, such as beads and glitter. The expanded pectin-containing biomass composition can be present in an amount from at or about 0.001% to at or about 2% by weight of the total weight of the composition.

H. METHODS FOR MODIFYING A PROPERTY OF A COMPOSITION

Provided are methods for modifying a rheo logical property of a composition. The modification can include increasing a viscosity, or modulating a yield stress. The methods include adding to the composition an amount of expanded pectin-containing biomass composition provided herein or an activated pectin-containing biomass composition having a coil overlap parameter of 2 or greater sufficient to increase the viscosity, or to modulate the yield stress. The amount of expanded pectin-containing biomass composition present can be in an amount from at or about 0.001% to at or about 2% by weight of the total weight of the composition. The amount of activated pectin-containing biomass composition present can be in an amount from at or about 0.01% to at or about 5% by weight of the total weight of the composition. The method can include preparing a concentration of activated pectin-containing biomass composition by dispersing the activated pectin-containing biomass composition in an aqueous medium or a portion of the fluid phase of a composition to yield a dispersion, adding the other components of the composition to the activated pectin-containing biomass composition dispersion to form a mixture, and subjecting the mixture to extensional stress to expand the activated pectin- containing biomass composition into the expanded pectin-containing biomass composition. The extensional stress can be applied to the mixture by applying high shear or passing the mixture through a high pressure homogenizer. The mixture can be passed

I , 2 or more times through the homogenizer. Provided are methods for altering a physical or processing property of a food, industrial, pharmaceutical, oilfield, household care, or personal care product. The methods include adding to the product an amount of expanded pectin-containing biomass composition provided herein or an activated pectin-containing biomass composition sufficient to alter a physical or processing property of the final product. The amount of expanded pectin-containing biomass composition present can be in an amount from at or about 0.001% to at or about 2% by weight of the total weight of the composition. The amount of activated pectin-containing biomass composition present can be in an amount from at or about 0.01% to at or about 5% by weight of the total weight of the composition. The method can include preparing a concentration of the activated pectin-containing biomass composition by dispersing the activated pectin-containing biomass composition in an aqueous medium or a portion of the fluid phase of the product to form a mixture, and expanding the mixture. The other components of the product can be added to the expanded mixture. The mixture can be stirred to uniformly distribute the components in the concentrate to yield the final product. The method can include as a step, after stirring to distribute the added components, subjecting the mixture to an additional extensional stress, such as by passing through a homogenizer. The extensional stress can be applied to the mixture by passing the mixture through a high pressure homogenizer. The mixture can be passed 1 , 2 or more times through the homogenizer. Alternatively, the activated pectin- containing biomass composition is dispersed into the liquid in the composition of the product, remaining ingredients are added, and the activated pectin-containing biomass composition is expanded during the heat treatment of the product, by up or down stream homogenization as appropriate for the process.

Provided are methods for reducing the caloric content of a prepared food product. The methods include replacing one or more of a fat, a sugar, or a starch with an amount of expanded pectin-containing biomass composition provided herein or an activated pectin- containing biomass composition having a coil overlap parameter of 2 or greater sufficient to yield a final product having commercially acceptable physical and processing characteristics as the non-modified version of the prepared food product. The amount of expanded pectin-containing biomass composition present can be in an amount from at or about 0.001% to at or about 2% by weight of the total weight of the composition. The amount of activated pectin-containing biomass composition present can be in an amount from at or about 0.01% to at or about 5% by weight of the total weight of the composition. The method can include preparing a concentration of activated pectin-containing biomass composition by dispersing the activated pectin-containing biomass composition in an aqueous medium or a portion of the fluid phase of the product to form a mixture and expanding the mixture to produce a mixture containing the expanded pectin-containing biomass composition. The other components of the food product can be added to the expanded mixture. The mixture can be stirred to uniformly distribute the components in the expanded mixture to yield the final product. The method can include as a step, after stirring to distribute the added components, subjecting the mixture to an additional extensional stress, such as by passing through a homogenizer. The extensional stress can be applied to the mixture by passing the mixture through a high pressure homogenizer. The mixture can be passed 1, 2 or more times through the homogenizer to form processed mixture. The processed mixture then can be packaged, cooked, fried, retorted or further processed as necessary to yield the prepared food product.

I. EXAMPLES

The following examples are included for illustrative purposes only and are not intended to limit the scope of the embodiments provided herein.

Example 1. Preparation of activated pectin-containing biomass composition

Fresh orange peel was washed in alcohol using the methods described in U.S. Patent No. 8,323,513 and then pressed by hand, followed by a second consecutive wash/press, and dried to form a dry alcohol washed starting pectin-containing biomass composition. The material was comminuted to pieces of 10 mm or less at its largest diameter.

1,000 grams (dry matter) of alcohol washed starting pectin-containing biomass composition was treated with a activating solution comprising an aqueous acidic alcohol solution by contacting the material at 70°C for 1 hour under mechanical energy of 10,800 kilojoules to convert the protopectin into pectin or a pectinaceous material. The amount of acid that was used was selected to correspond to the amount of acid used in a dry peel extraction (0.1 mL acid/gram peel): 1000 gram dry peel, 100 mL 62% nitric acid; 30 L 60% isopropyl alcohol.

The mechanical energy was induced by constant recirculation pumping of the sample mixture (biomass, alcohol, and acid) at 5,200 L/hr from a vessel (KOFA ApS, volume 25 L) through a tube heat exchanger (3 meters in length; 6" outer diameter; 2 inner tubes, each with a diameter of 1½") and back to the vessel using a lobe pump (APV, CL/1/021/10) that operated at 50 Hz. After being activated and fibrillated by exposure to the mechanical energy of the pump, the sample mixture was cooled to 15°C and then was drained using a Vincent press (model CP-4). The drained sample was then washed twice, where each wash was for 5 minutes in 30 L 60% isopropyl alcohol with a pH adjustment to 3.5 using 10% sodium carbonate. The washed sample was then dried in a heat cabinet at 65°C for 10 hours. The dried sample was then milled to a particle size of 250 microns, yielding Example 1 A.

The recovery (% of soluble pectin within the sample), the intrinsic viscosity (of the pectin extracted from the sample), residual sugar content (% by weight of the sample), degree of esterification of the pectin in the sample (DE), degree of galacturonic acid of the sample (GA), and apparent viscosity (VIS) of the sample in a 2% solution/dispersion at pH 4, were measured. The test methods are described in detail in the Staunstrup Applications. The preparation was repeated using similar starting biomass, yielding products IB and 1C. The results are summarized in Table 1.

Table 1. Activated Pectin-containing Biomass Composition Data

The data demonstrates that pectin-containing biomass activated by exposure to the activating solution and fibrillated/re fined via exposure to mechanical energy via the lobe pump have a very good percentage of pectin recovery. This result was surprising as it was conventionally believed that exposing the starting pectin-containing biomass composition to mechanical energy of greater than 1,200 kilojoules per kg dry matter would break or disintegrate the material into a form that made separation of the activating solution, and also extraction of the pectin, therefrom more difficult, and therefore was expected to undesirably decrease pectin yield. The DE of the pectin indicates a high methoxy pectin. The activated pectin-containing biomass composition also had a coil overlap of 2.5 or more.

Example 2. Effect of Homogenization in an Aqueous System

An aqueous concentration of the activated pectin-containing biomass composition (PBC) prepared in Example 1 A was prepared by mixing with a propeller mixer at a speed of from 500 to 1000 rpm of a 0.25 wt% Example 1A powder dispersed in standard tap water (STW, which contains 1 g NaCl + 0.147 g CaCl₂-2H₂0 / liter of water) for about 30 minutes, resulting in a homogeneous dispersion. The dispersion then was subjected to repeated exposure to extensional stress applied by passing the concentration through a high pressure homogenizer (APV Gaulin, single stage) at 3,500 psi for 5 consecutive passes to produce an expanded pectin-containing biomass composition. The viscosity of the resulting suspension was measured at 3 rpm on a Brookfield LVDV++ viscometer (Middleboro, MA). The results are shown in Table 2 below.

Table 2. Effect of Homogenization on Viscosity

The data demonstrate that complete expansion of the expanded pectin-containing biomass composition at the concentration prepared and the pressure used for expansion was essentially achieved after 2 passes through a high pressure homogenizer, and that subsequent passes did not have a negative impact on the fiber network.

Example 3. Re-expansion after Dilution

The effect of dilution of an expanded pectin-containing biomass composition was evaluated. A 1% concentrate concentration of expanded pectin-containing biomass composition was prepared by dispersing 10 g activated pectin-containing biomass composition of Example 1 A in 990 mL STW and exposed to an extensional stress by passing the concentration through a high pressure homogenizer (APV Gaulin, single stage) at 3,500 psi using two passes. This concentrate was diluted using STW by adding the STW to achieve an expanded pectin-containing biomass composition level of 0.25%, mixing with a propeller mixer at 750 rpm. The viscosity of the propeller-mixed dispersion was recorded. The propeller-mixed dispersion then was homogenized using a single pass through the APV Gaulin homogenizer at 2,000 psi. The results are shown in Table 3. Table 3. Effect of Homogenization on Viscosity

The data demonstrate that, after dilution, such as when a concentration of expanded pectin-containing biomass composition is added to other components of a formulation, a mild re-expansion can be necessary to achieve full functionality of a diluted concentration of the expanded pectin-containing biomass composition.

Example 4. Golden Italian Herb Salad Dressing

An Italian Herb salad dressing was prepared using the activated pectin-containing biomass composition of Example 1 A. The formulation is provided in Table 4.

Table 4. Golden Italian Herb salad dressing formulation

To prepare the dressing, the sugar, salt and activated pectin-containing biomass were dry blended together. The dry blend was added to the water and vinegar, and the resulting mixture was mixed for 10 minutes using a propeller mixer. Then, the mixture was mixed on a Silverson rotor stator mixer for 1 minute. The resulting product then was homogenized twice in a Gaulin APV homogenizer at 3,500 psi. The spices and soybean oil then were mixed with propeller mixing into the homogenized product to yield the final dressing.

The dressing had a Brookfield viscosity of 1,200 mPa*s when measured at 6 rpm and 261 mPa*s when measured at 60 rpm using a #2 LV cylindrical spindle. The spices remained distributed throughout the aqueous phase and did not settle out upon standing. When shaken, the oil and water readily mixed to form a dressing having the expected pourability and cling. The emulsion separated upon standing, which is typical for a Golden Italian Herb dressing, which is a coarse emulsion and expected to separate.

A similar formulation to that shown in Table 4 was prepared to investigate the effect of different mixing equipment on the final viscosity of the dressing. The amount of activated pectin-containing biomass composition included in the formulation was increased to 0.4 wt%, and the water was decreased to 49.65%. Different mixing equipment was used on different batches of the same formulation to determine the effect of shear on the viscosity of the final product, which is an indication of efficiency of the mixing equipment on expansion of the activated pectin-containing biomass composition into the expanded pectin-containing biomass composition. One sample was prepared using a Scott mixer. One sample was prepared using a Silverson rotor stator mixer. One sample was prepared using a high pressure homogenizer (APV Gaulin, 3,500 psi, 2 passes). One sample was prepared by first pre-activating a concentration of the activated pectin-containing biomass composition in the aqueous phase of the dressing formulation, adding the oil and dry herb ingredients and homogenizing via 1 pass through the APV Gaulin homogenizer at 3,500 psi. For comparison, a dressing was prepared with 0.15 wt% Keltrol^® xanthan gum using normal mixing conditions. The results are shown in Table 5.

Table 5. Effect of Application of Shear on a Formulation

The data show that high shear mixing using a Scott mixer or a rotor stator mixing device such as a Silverson mixer does not fully extend the reticulated cellulosic network of the activated pectin-containing biomass composition, and thus full functionality is not achieved, but rheology modification is achieved. The application of a uniaxial extensional stress using the high pressure homogenizer extends the reticulated cellulosic network to form the expanded pectin-containing biomass composition. Full functionality also can be achieved if the activated pectin-containing biomass composition is expanded by high pressure homogenization into the expanded pectin-containing biomass composition before the dressing is fully assembled. When the activated pectin-containing biomass composition is expanded by high pressure homogenization before the dressing is fully assembled, the final viscosity of the dressing is similar to that achieved using xanthan gum.

Example 5. French Salad Dressing

A French salad dressing was prepared using an expanded pectin-containing biomass composition prepared by expanding the activated pectin-containing biomass composition of Example 1 A. The formulation is provided in Table 6.

Table 6. French salad dressing formulation

To prepare the dressing, the vinegar, salt, EDTA and HFCS were added to the water with mixing using a propeller mixer. The solution was mixed for a total of 5 minutes using the propeller mixer. Different amounts of activated pectin-containing biomass composition were included in each formulation, from 0.1 wt% to 0.35 wt% activated pectin-containing biomass composition (PBC), reducing the amount of water as appropriate. The activated pectin-containing biomass was dispersed into the liquid with propeller mixing, and the mixture was mixed for at least 10 minutes or until a uniform concentration was produced. The concentration then was homogenized twice on an APV Gaulin homogenizer at 3,500 psi to form the expanded PBC. The sodium benzoate, tomato paste, paprika oleoresin and vinegar were added to the homogenized product using a propeller mixer. The soy oil then was slowly added with mixing to form a coarse emulsion. The course emulsion then was emulsified in a colloid mill with a 0.01 gap to which a progressive cavity pump (Moyno pump, NOV Process & Flow Technologies UK Limited, Manchester, UK) was connected.

For comparison, a dressing was prepared with 0.3 wt% Keltrol^® xanthan gum using normal mixing conditions. The results are shown in Table 7.

Table 7. Effect of Application of Shear on Formulation

The data show that preparation of a dressing formulation with the expanded pectin- containing biomass resulted in a final dressing product that exhibited a viscosity achieved using xanthan gum at very favorable (almost comparable) use levels of expanded pectin- containing biomass.

Example 6. Ranch Salad Dressing

A ranch salad dressing was prepared using an expanded pectin-containing biomass composition prepared by expanding the activated pectin-containing biomass composition of Example 1A in the formulation in situ. The formulation is provided in Table 8.

Table 8. Ranch Dressing Formulation

Activated PBC 0.28 Garlic powder 0.50

Basil, dried sweet 0.07

White pepper 0.06

Potassium sorbate, 0.05

powdered

Calcium disodium 0.03

EDTA

Chives, dried 0.02

Total 48.67 Total 51.33

The water phase was prepared by dry blending the sugar, buttermilk powder and activated pectin-containing biomass composition, and the dry blend was added to the water with mixing using a propeller stirrer and mixed for 10 minutes. The vinegar, lactic acid, and lemon juice then were added, and the mixture was mixed using a Silverson rotor stator mixer for 1 minute to fully disperse the activated pectin-containing biomass composition. The dispersion then was homogenized twice on an APV Gaulin homogenizer at 3,500 psi. With constant mixing, the egg and oil slowly were added to create a coarse emulsion. The course emulsion then was emulsified in a colloid mill with a 0.01 gap to which a progressive cavity pump (Moyno pump, NOV Process & Flow Technologies UK Limited, Manchester, UK) was connected.

The dressing had a Brookfield viscosity of 9,050 mPa*s when measured at 6 rpm and 2,300 mPa*s when measured at 60 rpm using a #2 LV cylindrical spindle. The formulation was stable, with no visible separation after 7 days.

Example 7. Barbeque Sauce

A barbeque sauce was prepared using the expanded form of the activated pectin- containing biomass composition of Example 1A. The formulation is provided in Table 9.

Table 9. Barbeque Sauce Formulation

Soy bean oil 2.50

Sugar 13.00

Brown sugar 5.00

Onion powder 0.50

Liquid caramel color 0.10

Cayenne pepper 0.18

Cumin 0.20

Liquid smoke flavor (Wright's) 0.60

Garlic powder 0.25

Paprika 0.70

Total 100.00

The barbeque sauce was prepared by adding the water, vinegar and molasses to a container that can be heated. The activated pectin-containing biomass composition was added with mixing with a propeller mixer and the concentration was mixed for 10 minutes. The concentration then was mixed for 1 minute with a Silverson rotor/stator mixer to ensure dispersion of the activated pectin-containing biomass composition. The mixture was added to the container and, with constant mixing using a propeller mixer, the mixture was heated for a heating time of 10-15 minutes. After the mixture had begun to warm, the tomato paste, salt, oil, both sugars, caramel color, and spices were added. When the mixture reached a temperature of 80°C, the liquid smoke was added. At 92-95°C, the mixture was removed from the heat, and homogenized twice on an APV Gaulin homogenizer at 3,500 psi.

The dressing had a Brookfield viscosity of 39,500 mPa*s when measured at 6 rpm and 8,500 mPa*s when measured at 60 rpm using a #2 LV cylindrical spindle. The formulation was stable, with no visible separation after 7 days.

Example 8. Sweet and Sour Sauce

A sweet and sour was prepared using the expanded form of the activated pectin- containing biomass composition of Example 1A. The formulation is provided in Table 10.

Table 10. Sweet and Sour Sauce Formulation

Water 29.06

Activated PBC 0.80

Sugar, granular 25.00

Brown sugar 15.00

Vinegar, white 8.00

Lemon juice 3.00

Soy sauce 7.00

Red pepper 0.03

Garlic 0.03

Paprika 0.03

Ginger, powdered 0.04

Mustard Powder 0.03

Total 100.00

The sweet and sour sauce was prepared by adding the liquid ingredients, sugars and activated pectin-containing biomass composition to a container that can be heated. The activated pectin-containing biomass composition was added with mixing with a propeller mixer and the concentration was mixed for 10 minutes. The mixture then was heated with constant mixing using a propeller mixer until the mixture reached a temperature of 92-95°C, which took a total heating time of about 10-15 minutes. At 92- 95°C, the mixture was removed from the heat, and homogenized twice on an APV Gaulin homogenizer at 3,500 psi. The spices then were added with constant stirring and the sauce was allowed to cool to room temperature.

The dressing had a Brookfield viscosity of 18,200 mPa*s when measured at 6 rpm and 4,200 mPa*s when measured at 60 rpm using a #2 LV cylindrical spindle. The formulation was stable, with no visible separation after 7 days.

Example 9. Protein Interactions

The interaction of the expanded pectin-containing biomass composition was evaluated with several different proteins under varying test conditions using the Example 1C material. Interactions with egg white (standard spray dried powder, Sonstegard Foods Co.), soy protein (Solae XT40), whey protein (Kellogg Provone 272 whey protein isolate), sodium caseinate (180 from Fonterra) and whole milk (grade A, pasteurized and homogenized) were evaluated. A 3700 mL stock dispersion of 0.6% activated pectin-containing bio mass (moisture corrected basis) was prepared in STW and mixed for 15 minutes with a 50 mm diameter prop stirrer. The expanded pectin-containing biomass was further dispersed using a Silverson mixer for 2.5 minutes at 7000 rpm. Using gentle prop mixing, the dispersion was de-aerated for 10 minute (the slow mixing allowed any entrained air to rise). The dispersion was expanded using 3 passes through an APV Gaulin homogenizer (single stage, 3,000 psi) to produce an expanded pectin-containing biomass. The expanded pectin-containing biomass was deaerated using a prop mixer at low speed to remove air for 10 minutes.

The proteins were prepared at a 2% concentration in STW. The whole milk was used as received. Equal weights of expanded pectin-containing biomass and protein (300 g) were added to a blender jar for titration. 3 different HC1 concentrations were used, 0.41N for the sodium caseinate, whey and egg white proteins, 0.9N for the soy protein, and 2N for the whole milk. This was done so that the actual volume of acid added for the various proteins would provide similar dilutions. A blender speed setting of 7 (-13,500 rpm) provided the best balance of mixing without air entrainment. Mixing was done for 1 minute without adding acid and then the acid was added via titration as quickly as possible to a pH of about 3.9. Acid addition then was stopped, allowed to equilibrate for 10 seconds, and titration of additional acid was done to bring the pH to 3.8 + 0.01. The volume of acid added and the time of mixing were recorded.

Unadjusted pH samples were prepared using the procedure just described but, in place of the volume of acid added, STW was added to dilute the sample. This provided a sample with similar mix history and dilution but without a pH change. A control sample (no added protein) was prepared by diluting 1 : 1 with STW and following the dilution and mix times described above.

The effect of heat also was tested. A microwave oven was used to quickly heat the appropriate samples. The sample was transferred to a 300 mL beaker to minimize boil- over. Heating was stopped when the sample had just begun to boil (about 75 sec). The beaker was then removed and stirred before being heated an additional 15 seconds. Due to precipitation, the sodium caseinate was not tested at pH 3.8. Neither egg white sample was heated for the same reason. After the second heating cycle the sample was stirred, poured back into the original 200 mL tall form beaker and placed into an ice bath for cooling. After 1 minute in the ice bath the sample was stirred one more time. When the temperature dropped to 20°C the sample was removed from the ice bath and allowed to remain undisturbed for 30 minutes. For heated and unheated samples, viscosities were measured using a Brookfield LV viscometer. The viscometer was fitted with a #1 LV spindle and run 30 seconds at 30 rpm to pre-shear the sample, then 3 rpm for 60 seconds. The 3 rpm viscosity after 60 seconds was recorded.

It was determined that most of the viscosity in these expanded pectin-containing biomass systems (-650 mPa*s) comes from the cellulosic fiber component. Centrifuging out the soluble pectin provided a viscosity of 8.1 mPa*s or approximately 1.2% of the total system viscosity. Likewise, the viscosity of the proteins at the concentrations used in this test was essentially insignificant. The values ranged from 1.05 mPa*s for egg white to 1.49 mPa*s for whole milk. Accordingly, changes in viscosity when protein was added to the expanded pectin-containing biomass system could be attributed predominately to changes in the reticulated cellulosic fiber network of the expanded pectin-containing biomass composition.

A decrease in viscosity could come from destabilization of the reticulated cellulosic network due to aggregation. Such aggregation can arise when the co-agent function of the associated pectin is compromised. This can lead to decreased cellulosic surface area and the concomitant drop in measured viscosity. On the other hand, a viscosity increase can be attributed to a filling in of the cellulosic network with protein in a particulate (non-soluble) state. Since dropping the pH and/or heating tends to make proteins precipitate, those small protein particles fill in the pores of the cellulosic network and thus make the network stronger. Such a reinforced network will resist shear flow more effectively and increase measured viscosity. The data is shown in Table 11.

Table 11. Protein Interactions

Whey powder 877 33.6

Whey powder heated 867 31.9

Whey powder pH 3.8 635 -3.20

Whey pH 3.8 & heated 593 -9.60

Whole milk 977 48.8

Whole milk heated 811 23.4

Whole milk pH 3.8 1059 61.5

Whole milk pH 3.8 & heated 733 11.7

The data show that soy protein at its native pH in the presence of expanded pectin- containing bio mass enhanced the cellulosic network. The interaction of the soy protein with the pores of the reticulated cellulosic fiber network of the expanded pectin-containing biomass composition resulted in a stronger network, indicated by a higher viscosity. This reinforcement remains even when the same is heated. Reducing the pH changed this substantially. Before heating, the sample containing expanded pectin-containing biomass composition with soy protein adjusted to pH 3.8 had a similar viscosity to the sample containing expanded pectin-containing biomass composition alone. When heated, the sample containing the soy protein and the expanded pectin-containing biomass composition at pH 3.8 demonstrated a substantial viscosity drop, indicating an adverse effect.

Egg white also was able to enhance the reticulated cellulosic network of the expanded pectin-containing biomass composition at neutral pH but showed less interaction when the pH is lowered. No tests could be done with the egg white after heating, as the dispersions were completely flocculated. Sodium caseinate was not very soluble at neutral pH but it was compatible with the reticulated cellulosic network of the expanded pectin- containing biomass composition and enhanced the system viscosity. When heated, the caseinate proteins were further denatured and are not as effective in enhancing viscosity. Reducing the pH to 3.8 without heating resulted in roughly a 40% boost in viscosity of the combined system. However, when heated, the system became two phases and no meaningful measurements of viscosity were possible.

Whey protein at an unadjusted pH was more soluble than casein and an enhancement of viscosity of the expanded pectin-containing biomass composition plus whey protein system was observed. The observation held even after heating if the pH was not adjusted. Overall, the protein components of whey have a net negative charge at this pH. Lowering the pH to 3.8 resulted in the whey protein having a net positive charge and the effect on expanded pectin-containing biomass composition plus whey protein suspension was evident. The system was less stable and was lower in viscosity. Applying heat along with the lower pH resulted in a substantial drop in viscosity due to both the charge on the protein as well as the denaturation occurring due to heat.

With an unadjusted pH, the sample containing whole milk and the expanded pectin-containing biomass composition exhibited enhancement of the viscosity. The enhancement decreased some with heating. Lowering the pH meant that some of the proteins were destabilized and the samples showed a large variation from one repeat test to another. Further denaturation with heat intensified the effect and led to both less viscosity and a physical appearance that was coarse and somewhat grainy.

Example 10. Hydrocolloid Interactions

The interaction of the expanded pectin-containing biomass composition was evaluated with several different hydrocolloids under varying test conditions using the expanded form of the activated pectin-containing biomass composition of Example 1C. Interactions with xanthan gum, modified instant starch, and unmodified corn starch were evaluated.

The activated pectin-containing biomass composition of Example 1C was dispersed in standard tap water using propeller mixing at 750 rpm for 1 hour until the fiber was well dispersed to form a concentration. The concentration of the activated pectin- containing biomass composition was expanded by using two passes through an APV homogenizer at 3,500 psi.

KELTROL® xanthan gum was prepared using 1 hour of propeller mixing at 750 rpm to have a shear viscosity of 100 mPa*s (Brookfield 3 rpm, #1 spindle) in standard tap water. This was a concentration of 0.11%.

Modified instant starch (Ingredion, Instant Clearjel) was prepared using 1 hour of propeller mixing at 750 rpm to have a shear viscosity of 100 mPa*s (Brookfield 3 rpm, #1 spindle) in standard tap water. This was a starch concentration of 3.78%.

An unmodified corn starch suspension was prepared using 1 hour of propeller mixing at 750 rpm in standard tap water at the same concentration as the modified starch (3.78%). The starch concentration was kept constant in order to compare pre-gelatinized starch with an uncooked native starch.

For all three samples, a 1 : 1 blend was made and homogenized 1 additional pass through a custom designed extensional homogenizer at 1,500 psi (roughly equal to a conventional homogenizer at 2,500 to 3,000 psi). At the same time a control was prepared by dilution of the activated pectin-containing biomass composition (PBC) with standard tap water. The results are shown in Table 12.

Table 12. Results of Hydrocolloid Interactions with Expanded PBC

These results show that the expanded pectin-containing biomass composition in the presence of a hydrocolloid exhibits a synergistic increase in viscosity (the resulting viscosity is not additive) compared to the expanded pectin-containing biomass composition alone. When modified starch is added to the expanded pectin-containing biomass composition, the starch fills in the pores of the reticulated cellulosic fiber network of the expanded pectin-containing biomass composition and provides a viscosity enhancement that is substantial. There is a moderate increase in the viscosity when a water-soluble polymer like xanthan gum is added, but the synergism with the modified starch is considerably greater. When the starch granules have not been cooked or expanded by heating, there is very little enhancement of the viscosity. An explanation for this is that the swollen instant starch can provide reinforcement of the reticulated cellulosic network of the expanded pectin-containing biomass composition and thus makes it higher in shear viscosity.

Example 11. Yogurt Fruit Preparation - Expanded PBC

Yogurt fruit preparations were prepared using the activated pectin-containing biomass composition of Example IB that was expanded by exposure to an extensional stress. The expanded pectin-containing biomass composition was compared to a comparable pectin having a similar %DE. The activated pectin-containing biomass composition of Example IB was found to have an average of about 35% pectin and a %DE of about 71. Therefore, the tests were performed in yogurt fruit preparation formulations comparing the activated pectin-containing biomass composition with GENU^® pectin type B rapid set, with a similar %DE (GENU® pectin type LM-102-AS). The formulation is provided in Table 13. Table 13. Yogurt Fruit Preparation Formulation

*X is the pectin or expanded pectin-containing bio mass composition use level. (0.5 wt%, 1 wt% or 1.5 wt%)

The fruit, sucrose, sodium citrate, and water (A) were weighed, transferred to a cooking pan, heated to boiling with stirring, and boiled until soluble solids reading was 40%. The pectin or the activated pectin-containing biomass composition of Example IB and the sodium citrate were mixed into the hot (60°-80°C) water using a high speed mixer (7500 rpm for 5 minutes), and the resulting concentration was subjected to extensional stress by running it through a single stage homogenizer at 350 bar, one pass. The homogenized material was added to batch (A) and mixed well. The solids were adjusted to 40%). The samples were cooled to approx 40°C and filled into 1 liter glass beakers, and two back-extrusion plastic cups (100 ml in each cup). The glass beaker for each sample was maintained at room temperature and the plastic cups were maintained at 40°C overnight. Bostwick measurements (CSC Central Scientific Co., Inc., Fairfax, VA), which measure a distance a specific volume of product flowing in a centimeter graded flow chamber, after 10, 30 and 60 seconds were recorded. The samples also were subjected to a back-extrusion test using a Stable Micro Systems: TA.TX.plus Texture Analyser, load cell 5 kg fitted with 50 mm back-extrusion rig and 40 mm disc to measure thickening effects. The samples also were subject to stability evaluations. The data are show in Table 14.

Table 14. Bostwick, Texture and Stability Data

10 >23 >19 15 19 11 6.5

30 - 23 19 21 12 7.0

60 - 23 21 22 12 7.5

Back-extrusion

Energy used, g*mm 285.6 391.6 404.3 354.3 664.6 1282

No - Fruit No - Yes No - Yes Yes

Stable (Yes/no) sediment thin at top thin at top

The samples containing GENU pectin B rapid set at the usage levels shown do not provide the same stability, nor viscosity as the expanded pectin-containing biomass composition provided herein. The Bostwick, and the back-extrusion values, are similar for 1.0% GENU^® pectin B rapid set sample and the 0.25% expanded pectin-containing biomass composition sample, but neither formulation was judged to be stable due to thinning at the top of the formulations. The sample containing 1.5% GENU^® pectin B rapid set produced a stable formulation, but the Bostwick value was too high (above 15 cm at 10 seconds), and the viscosity was too thin. In comparison, the sample containing 0.5% expanded pectin-containing biomass composition produced a stable formulation with a Bostwick value of 11cm, which is a bit on the high side. Samples containing 1.0% expanded pectin-containing biomass composition exhibited a very gelled texture and were judged difficult to stir the fruit part into a yogurt. Accordingly, a use level of approximately 0.75% expanded pectin-containing biomass composition might be a more appropriate use level at these process conditions for production of a yogurt fruit preparation.

Example 12. Yogurt Fruit Preparations - Activated PBC

Yogurt fruit preparations were prepared using the activated pectin-containing biomass composition of Example 1A. The activated pectin-containing biomass composition was compared to a comparable pectin having a similar % DE. An activated pectin-containing biomass composition produced as described in Example 1A was found to have an average of about 39% pectin and a % DE of about 68. Therefore, the tests were performed in yogurt fruit preparation formulations comparing the activated pectin- containing biomass composition with GENU^® pectin type B rapid set, with a similar %DE (GENU® pectin type LM-102-AS, batch SK 721 11). The formulation is provided in Table 15. Table 15. Yogurt Fruit Preparation Formulation

¹ Modified starch = Thermflo (batch GFU501J, Ingredion)

The fruit, sucrose, sodium citrate, and water (A) were weighed and transferred to a cooking pan. The components of (B) were dry blended and dispersed into the (A) components for the reference sample (ref), and sucrose only was dispersed into the (A) components for the activated pectin-containing biomass composition (PBC) sample, while stirring with a wooden spoon. This mixture was heated to boiling and held for 5-10 minutes while gently stirring.

The pectin or activated pectin-containing biomass composition separately was dispersed in hot (60-80°C) water (C) using a high-speed mixer (7,500 rpm for 10 minutes) to dissolve pectin, or to disperse the activated pectin-containing biomass composition. The solids level of both solutions was adjusted to 40%. The samples were cooled to approximately 40°C and filled into 1 -liter glass beakers, and two back-extrusion plastic cups (100 ml in each cup). The glass beaker for each sample was maintained at room temperature and the plastic cups were maintained at 40°C overnight.

Sensory evaluation of the samples showed that the reference sample thickened with modified starch and pectin had lots of body, a typical spoon test and mouthfeel, and was more viscous than expected. The sample thickened with the activated pectin- containing biomass composition had a smooth and coherent texture, and had more resistance in the spoon test, results that were closer to the standard.

The samples in the back-extrusion plastic cups were measured using a TA.TX.plus Texture Analyser with a load cell 5 kg fitted with 50 mm back-extrusion rig. The device presses a plunger through the surface and then pulls the plunger out of the sample. The data is useful to illustrate the texture differences observed between samples. The device calculates the work (force x distance) done to press the probe down through the sample as well as the work done to lift the probe out of the sample. The data are shown in Table 16.

Table 16. Bostwick and Texture Data

The activated pectin-containing biomass composition sample exhibited a similar texture as the sample prepared with pectin/starch. Bostwick values of the sample containing the activated pectin-containing biomass composition sample were slightly higher but were in the normal range. When stirred into yogurt, the sample containing the activated pectin-containing biomass composition sample was similar to the sample prepared with pectin/starch, being easy to stir into the yogurt with a spoon. After storage at 1 hour at 5°C, both samples were smooth, with a homogeneous appearance and an even distribution of fruit preparation. No sedimentation or syneresis was observed. Neither of the samples exhibited curdling. Accordingly, the activated pectin-containing biomass composition sample easily replaced the pectin product and created a similar fruit texture and ease of use in the yogurt preparations.

Example 13. Stabilizing Emulsions

The ability of the activated pectin-containing biomass composition to stabilize an oil- in- water emulsion was evaluated. The emulsion stability abilities of the fibers were explored using different shear applied during the emulsion preparation process using medium shear (Silverson L4Rt rotor stator mixer with general purpose disintegrating head, 1.5 cm holes, 7,000 rpm) and high shear (homogenizer, Rannie type 12.50, 200/50 bar two stages, or 300/50 bar (double homogenization). The homogenizer converted the activated pectin-containing biomass composition into an expanded pectin-containing biomass composition in situ.

Comparative studies were performed and included as an ingredient either

HERBACEL® AQ® PLUS Citrus or GENU pectin B rapid set pectin. HERBACEL® AQ® PLUS Citrus (H.AQ P) is a citrus fiber from Herbafood Ingredients GmbH, Werder (Havel), Germany H,AQ P contains about 10% pectin. GENU pectin B rapid set pectin is a pectin that is similar to the pectin component of the activated pectin-containing biomass composition and expanded pectin-containing biomass composition.

The activated pectin-containing biomass composition was the material of Example 1C. For these studies, a medium hard water with approx 10°dH was used, prepared by blending tap water (20°dH) 1 : 1 with de-ionized (DI) water. The activated pectin-containing biomass composition is flexible with respect to the order of addition of ingredients, and no important differences were observed when the fiber composition was added to cold oil, to cold water, or to a mix of both. For these studies, the fiber composition was added to the oil to create a concentration. Emulsions containing 20%, 40% and 60% rapeseed oil were prepared using medium and high shear and 0.75% of Example 1C activated pectin- containing biomass composition.

Emulsions were prepared using a cold preparation process. The test thickener was dispersed in the oil using the propeller stirrer, 500 rpm, 2 min. The cold water was added and stirring was continued for 10 min. The sample was divided into two aliquots. One was subjected to medium shear using the Silverson rotor stator mixer at 7,000 rpm for 10 min. The other aliquot was subjected to extensional shear using the homogenizer at 200/50 bar, two stages, resulting in in situ formation of the expanded pectin-containing biomass composition. Samples of 250 mL from each preparation were collected in plastic cups and placed in cold storage. Viscosity measurements and sensory evaluations were performed after 1 day (D+l) and after 5 days (D+5). Viscosity was measured using a Brookfield viscometer mounted on a helipath drive motor and a T-bar spindle was used to create a helical path through the emulsion. Sensory evaluations included visual evaluation of emulsion stability, appearance and texture. The results are shown in Table 17. Table 17. Test Results of 0.75% Activated PBC with Medium and High Shear

Samples prepared using medium shear (Silverson) have acceptable viscosities and appearances, with thin, pourable textures. The sample containing and with 0.75% activated pectin-containing biomass composition the sample with 20% oil is stable, but samples with higher oil levels show instability. Stability of the emulsion with 40% and 60% oil can be improved by increasing the activated pectin-containing biomass composition use level, compensating for lower expansion of the fiber using medium shear.

Samples prepared using the homogenizer, which resulted in production of the expanded pectin-containing biomass composition in situ, exhibited good emulsion stability with 0.75% fiber usage. The viscosity measurements were much higher than those achieved using medium shear, and as expected the viscosity increased with increasing oil and decreasing water content. The samples exhibited a spoonable, slightly gelled texture. The emulsions had a shiny and smooth appearance, and they were stable after 1 month of cold storage.

Samples were prepared using the high shear homogenization using the same procedure as described above, except that 0.75% HERBACEL® AQ® PLUS Citrus fiber (H.AQ) was used to prepare oil-in-water emulsions with 20%>, 40%> and 60%> rapeseed oil. The results are shown in Table 18. For comparison, the test results for the activated pectin- containing biomass composition (aPBC) shown in Table 18 above are included. Table 18. Test Results of Emulsions Containing 0.75% H.AQ

Samples containing 0.75% HERBACEL® AQ® PLUS Citrus fiber that were homogenized were not stable. Compared to corresponding samples containing 0.75%> expanded pectin-containing biomass composition, the viscosity levels of the H.AQ samples are significantly lower, especially for the samples with 40%> and 60%> oil, caused by unstable emulsions leaking oil. Even the 20% oil emulsion appeared unstable.

Additional testing of H.AQ in 40% oil-in-water emulsions, prepared by activating the H.AQ in cold water also failed to produce a stable emulsion. Emulsions prepared using 0.75% HERBACEL® AQ® PLUS Citrus fiber subjected to medium shear using the Silverson rotor stator mixer at 7,000 rpm for 10 min. yielded an unstable, inhomogeneous mixture, while a comparable amount of activated pectin-containing biomass composition exposed to the same shear conditions produced a stable emulsion. Thus, HERBACEL® AQ PLUS Citrus exhibited very poor emulsifying abilities in formulations of the test conditions compared to the expanded pectin-containing biomass compositions provided herein in the same formulations.

Activated pectin-containing biomass compositions and expanded pectin-containing biomass compositions were compared to GENU pectin B rapid set pectin for their ability to stabilize oil-in-water emulsions containing 40% oil, where the stabilizer use level was 0.25%), 0.5%) or 0.75%>. A cold make-up procedure as described above was used. In addition, a hot make-up procedure also was used. The hot make-up procedure included dispersing the stabilizer into cold oil while stirring with a propeller stirrer, at 500 rpm, for 1 min. The vessels containing the mixture then was placed under the Silverson rotor stator mixer, and the water (previously heated to 80°C) was added with mixing at 3500 rpm for 2 min. The mixture was heated to 80°C in a 85°C water bath with a propeller stirrer. Any water lost to evaporation during processing was added back using DI water. The mixture then was run through the homogenizer at 200/50 bar, two stages.

GENU pectin B rapid set pectin was not capable of stabilizing 40% oil-in-water emulsions at a usage level or 0.5% or 0.75%, neither with medium shear or high shear applied, nor when prepare with cold or hot expansion. All the GENU pectin B rapid set pectin emulsions were unstable, as they were separated with thin, pourable textures.

The test sample containing 0.75% activated pectin-containing bio mass composition prepared using cold expansion exhibited stable emulsions when prepared using medium shear and using homogenization. When the samples were prepared using hot expansion, 0.5% and 0.75% activated pectin-containing bio mass composition stabilized the emulsions prepared using homogenization, but only the sample with 0.75% activated pectin-containing biomass composition exposed to medium shear was able to stabilize the emulsion. The viscosity of emulsion samples prepared using homogenization, whether cold or hot, were significantly higher (by about 6 to 10 times), compared to the viscosity of the emulsion samples prepared using medium shear (Silverson rotor stator mixer). When comparing emulsions containing 0.75% activated pectin-containing biomass composition prepared using cold and hot expansion, slightly higher viscosities were achieved for cold expansion than for hot expansion, but no differences were observed in emulsion stabilities.

Example 14. Stabilizing Emulsions in Low Shear Applications

The ability of 2.0% or 2.5% of the activated pectin-containing biomass composition of Example 1A to stabilize food emulsions prepared using low shear (whisk) or medium shear (Silverson rotor stator mixer) in food prepared with a cold or hot makeup procedure was evaluated. For the hot make-up procedure, a bearnaise sauce formulation was used. The formulations used are shown in Table 19.

Table 19. Bearnaise Sauce Formulation.

SLENDID 120, GENU pectin 0.50 — —

SIMPLESSE 100, whey protein 1.00 ~ ~

concentrate

Maltodextrin 2.00 — —

Modified starch 2.50 — —

Skimmed milk powder 1.00 1.00 1.00

Sucrose 2.00 2.000 2.00

Onion powder 0.05 0.05 0.05

Salt/pepper 1.50 / 1.50 / 0.02 1.50 / 0.02

0.02

Tarragon, dried 0.10 0.10 0.10

Butter 10.00 10.00 10.00

Vinegar (7% acetic acid) 3.50 3.50 3.50

bearnaise essence 1.00 1.00 1.00

Egg yolk paste 5.00 5.00 —

Water (1 :1 tap:DI) - 69 - 73 - 78

In the formulation above, the KELTROL® AP xanthan gum provides texture, stability and mouthfeel to the formulation and enhances the emulsion stability. The SLENDID® 120 pectin and the SIMPLESSE® 100 whey protein concentrates mimic fat and enhance a creamy, fat-like mouthfeel. The formulation has a very smooth and creamy texture. The test formulation was prepared to determine whether the activated pectin- containing biomass composition could replace the starch, xanthan gum, pectin, whey protein concentrate and egg yolk to yield a stable emulsion with the same texture and mouthfeel.

The sauce was prepared by hand mixing the dry ingredients (except the salt and tarragon) into the water using a whisk. The melted butter slowly was added while stirring with a whisk, and once incorporated, the bearnaise essence, vinegar and salt were added while stirring with a whisk. For the formulation containing egg yolk, a portion of the sauce was removed and mixed with the egg yolk at a 1 :2 weight ratio and the egg yolk mixture was saved in a separate container. The rest of the sauce then was heated to 80- 90°C in a water bath while stirring with a whisk. For the formulation containing egg yolk, the egg yolk mixture was added while mixing with the whisk. The mixture then was reheated to 80-90°C in a water bath while stirring and the dried tarragon was added. A portion was removed (whisk mixed) and placed in a sample jar. The remaining mixture was mixed using a Silverson rotor stator mixer at 7,000 rpm for 5 min. and the resulting sauce was placed into sample jars.

Samples prepared using 2.5% of the activated pectin-containing biomass composition and whisk-only mixing produced a stable emulsion that was spoonable, with a texture that was less structured than the control but with a lower viscosity than the control. Samples prepared using 2.0% of the activated pectin-containing biomass composition and whisk-only mixing produced a stable emulsion but the viscosity was low. Samples prepared using 2.5% of the activated pectin-containing biomass composition and Silverson mixing produced a stable emulsion that was spoonable, with a texture that was more structured than the control but with a higher viscosity than the control. Samples prepared using 2.0% of the activated pectin-containing biomass composition and Silverson mixing produced a stable emulsion with a texture and viscosity similar to the control. The results showed that activated pectin-containing biomass composition can be able to replace stabilizers, starch, maltodextrin and egg yolk and produce a produce with a similar texture and mouthfeel. The usage level of the activated pectin-containing biomass composition can be adjusted according to the required viscosity and shear.

Comparable formulations using HERBACEL® AQ® PLUS Citrus fiber, FibreGel LC Citrus fiber (Florida Food Products, LLC, Eustis, FL), and Citri-Fi 100 FG, Citri-Fi 100 M40, and Citri-Fi 125 M40 citrus fibers (Fiberstar, Inc., River Falls, WI) were prepared for comparison. Each of fibers were used at 2.5% usage levels for the whisk- only and Silverson mixer preparations.

For formulations prepared using whisk-only mixing, FibreGel LC, Citri-Fi 100 FG, Citri-Fi 100 M40, and Citri-Fi 125 M40 where unstable and separated. The HERBACEL® AQ® PLUS Citrus fiber produced a stable product having a Brookfield viscosity of 14.97 mPa*s having a porridge-like appearance. The sample containing the activated pectin-containing biomass composition was stable, had a Brookfield viscosity of 10.06 mPa*s, and had a smooth shiny appearance.

For formulations prepared using Silverson rotor stator mixing, the samples containing FibreGel LC were unstable, exhibiting separation on the top of the sample and a very low viscosity. Samples containing Citri-Fi 100 FG were unstable, exhibiting separation on the bottom of the sample and a low viscosity. Samples containing Citri-Fi 100 FG, Citri-Fi 100 M40, and Citri-Fi 125 M40 citrus fibers were stable but had low viscosities. The HERBACEL® AQ® PLUS Citrus fiber produced a stable product having a Brookfield viscosity

The HERBACEL® AQ® PLUS Citrus fiber produced a stable product having a Brookfield viscosity of 106.9 mPa*s having a dull appearance, with a short texture and less mouthfeel than the control. The sample containing the activated pectin-containing biomass composition was stable, had a Brookfield viscosity of 98.75 mPa*s with a smooth shiny appearance, and a texture and mouthfeel more like the control.

For the cold make-up procedure, a Thousand Island salad dressing formulation was used to prepare test samples. The samples were mixed using a Silverson rotor stator mixer. A sample of activated pectin-containing biomass composition (Example 1C) was compared to HERBACEL® AQ® PLUS Citrus fiber at a usage level of 1.5% fiber. The formulation is provided in Table 20.

Table 20. Thousand Island Salad Dressing Formulation

The emulsion was prepared by adding the skimmed milk powder to the water using the Silverson mixer at 7,500 rpm for 2 min. Separately, the fiber, pepper, paprika, garlic powder and sugar were combined with the oil to form a blend. The oil blend then was added with mixing at 7,500 rpm to the milk mix and mixing continued for 5 minutes. The remaining ingredients were blended together and added to the mixture with mixing at 7,500 rpm and mixing continued for 1 minute. The samples were placed in sample storage gels and refrigerated overnight. The results are shown in Table 21.

Table 21. Test Results of Thousand Island Dressing Emulsions

The activated pectin-containing biomass composition (Example 1C) and the

HERBACEL® AQ® PLUS Citrus fiber at a usage level of 1.5% fiber can replace pectin, starch and egg yolk in a Thousand Island salad dressing and yield a stable formulation. The measured viscosity is higher in the sample containing the HERBACEL® AQ® PLUS Citrus fiber, but this sample has a dull surface appearance and looks like porridge. Repetitions with the same batch of HERBACEL ® AQ® PLUS Citrus fiber also resulted in emulsions having different viscosities, while the activated pectin-containing biomass composition (Example 1C) produced emulsions having very similar viscosities.

The activated pectin-containing biomass composition (Example 1C) performance depends on use level and the amount of shear using during preparation. At higher use levels, the activated pectin-containing biomass composition can provide stability/viscosity with lower shear, such as with a Silverson mixer. Homogenization results in the extension of the cellulosic fiber and creates an extended pectin-containing biomass composition in situ and maximizes activity. The activated pectin-containing biomass composition can replace stabilizers, starch, and egg yolk in dressings and can provide similar textures and mouthfeel in such formulations.

Example 15. Acidified Protein Drinks

Acidified protein drinks, such as yogurt drinks, directly acidified protein drinks, plant-based protein drinks, fermented and whey-juice drinks are a growing segment, as consumers select these beverages because of their health benefits. Pectin often is used to provide stabilization, thickening and suspension. Tests were conducted to demonstrate the functionality of the expanded pectin-containing biomass composition, which can be expanded either pre-processing and/or during processing, provided herein in acidified protein drinks. The activated pectin-containing biomass composition of Example 1C was used to produce the expanded pectin-containing biomass composition in situ in the final product. Comparable drinks were prepared with HERBACEL® AQ® PLUS Citrus Fiber (H.AQ), and GENU® pectin type YM-115-L for comparison. The formulation used is provided in Table 22. Table 22. Recipe for Yoghurt Drink with 1% Protein and 0.09% Fat

The following samples were prepared: 1) a control with no stabilizer added; 2) a reference with 0.3% GENU pectin type YM-115-L (YM); 3) a drink containing activated pectin-containing biomass composition of Example 1C (PBC) at a use level of 0.2-0.6% used alone, 3) a drink containing PBC at a use level of 0.2-0.4% combined with 0.3% YM; 4) a drink containing HERBACEL® AQ Plus (H.AQ) at a use level 0.4% use level, and 5) a drink containing H.AQ at a use level of 0.4% combined with 0.3% YM.

The drinks were prepared as follows. The fiber and/or pectin was dispersed in a portion of the DI water at 80°-85°C using a Silverson L4RT rotor stator mixer at 4,000- 5,500 rpm for 10 minutes. The concentrated dispersions contained 1.5% fiber. The pectin only was made as a concentrate at 2%. For the fiber dispersions, whether PBC or H.AQ, the dispersions were homogenized using a Rannie type 12.50 homogenizer at 350 bar, and the homogenized solutions then were cooled to 5°C. The yogurt, sugar and remaining DI water were mixed together using a propeller stirrer (IKA Eurostar digital) for 5 min. The YM (a HM pectin) was added and the mixture was stirred for 5 min. The homogenized fiber dispersion then was added to the mixture and stirred with a propeller stirrer for 10 min., and then stirred using a Silverson rotor stator mixer at 4,000 to 6,000 rpm for 5 min. The pH was checked and adjusted to pH 4, and a few drops of antifoam was added.

The mixture was transferred for processing using a MicroThermics aseptic processor (MicroThermics, Inc., Raleigh, NC). The mixture was homogenized at ambient temperature at 200/50 bar two stage, pasteurized at 90°C for 15 sec, cooled, and filled into bottles at 20°C. For stability testing, bottles were maintained at 5°C, room temp (about 25°C), and at 40°C. Visual and sensory evaluations were made after 7 and 35 days and 6 months of storage confirming shelf life stability.

Only minor differences were observed between samples kept at the different storage temperatures. The drinks containing 0.4% expanded PBC or HERBACEL® AQ Plus Citrus product, with or without added pectin, had similar viscosities and rheological profiles. The drink containing the HERBACEL® AQ Plus Citrus product, however, had a thinner, more watery mouthfeel than that of the drink containing the expanded PBC. The HERBACEL® AQ Plus Citrus drink also had a porridge-like appearance. The drinks exhibited a shear thinning behavior. Addition of pectin to the formulation containing the expanded PBC resulted in an increased viscosity. A formulation containing 0.2% expanded PBC and 0.3% high methoxy pectin was stable, having a smooth mouthfeel and good visual appearance.

The expanded pectin-containing biomass composition can stabilize acidified protein drinks. At a use level of 0.1 % to 1.0%, it produces a yogurt based acidified protein drink with no top whey separation or sediment. The expanded pectin-containing biomass composition provides good mouthfeel, more body, and less watery mouthfeel compared with HM pectin alone. Used together with 0.3% HM pectin, the viscosity increases and the particle size/instability index decreases. The mouthfeel and smoothness are improved as well due to less gelled/smaller particles.

Additional acidified protein drinks were prepared using samples of the activated pectin-containing biomass composition being prepared in accordance with the methods disclosed herein and having various coil overlap parameters. An ambient drinking yoghurt was prepared using an activated PBC from citrus fruit having a coil overlap parameter of 2.74 in the formulation as shown in Tables 23-24.

Table 23. Formulations of Ambient Drinking Yoghurt

GENU® Pectin LM-106 AS-YA 0.15% —

Water 11.00% 12.00%

Activated PBC — 0.60%

Total 100.00% 100.00%

The typical formula was prepared by dry blending modified food starch, agar, pectin and Simplesse® whey protein with sugar and adding to 55°C fresh milk while mixing for 15 minutes.

The activated PBC formula was prepared by first dispersing the activated PBC into water using a propeller mixer @ 600 rpm for 20 minutes and then expanding the activated PBC by using 2 stage homogenization @200/50 bar (3000/750 psi). Separately, Simplesse® whey protein was dry blended with sugar and added to 55°C fresh milk while mixing for 15 minutes. The expanded PBC was then added to the mixture of other ingredients using a propeller mixer until uniformly dispersed.

Both formulas were homogenized at 60°C, 200/20 bar (3000/300 psi), pasteurized in water batch at 85°C for 10 minutes, and cooled to 43°C and then culture added. The formulas were then incubated at 43°C for ~6 hours or until pH 4.4. The curd was broken using a frame agitator @ 150rpm for 3 to 5 minutes. The yogurt was cooled to 10°C and store refrigerated. The yogurt was then brought to ambient temperature and processed via UHT at 75°C for 30 seconds and then cooled to 25°C and aseptically fill into desired packaging. Storage was at ambient temperature.

It was observed that the expanded PBC can be used to replace modified food starch and agar. The finished beverage had a lighter mouthfeel and was stable over the shelf life tested.

Table 24. Formulations of Short Shelf Life Yoghurt Drink

The final product had 10-20%) of a 1%> PBC concentration, which provided 0.1-0.2%> expanded PBC in final yoghurt drink. Higher use level can provide higher viscosity and stability. The yoghurt base consisted of skimmed milk powder and de-ionized water. The final product was prepared using a high shear mixer (Silverson rotor stator mixer) and homogenizer as follows: weigh out water for 1% activated PBC concentration, disperse activated PBC into water (80-85 °C) using high shear mixer at 5000 rpm for 10 minutes, expand activated PBC using homogenizer single stage ( 350 bar), cool to ambient temperature and blend with yoghurt base, sugar and remaining water using high sear mixer at 3000 rpm for 5 minutes, homogenize single stage (180-200 bar), cool to below 10 °C, fill into bottles, and store at 5 °C until consumption.

Example 16. Yoghurt White Mass

Yoghurt white mass prepared using activated PBC (activated citrus fiber having a coil overlap parameter of 2.74) and compared with typical ingredients and processes for preparing conventional yoghurt white mass. The low- fat yoghurt had approximately 3.3% protein and 1% fat. Formulations were prepared using 0.3 to 0.9% activated PBC or alternatively starch/gelatin (1.25% THERMTEX / 0.5% 250 bloom type A), low methoxy pectin (0.20%> LM-18 CG-YA, CP Kelco ApS, Denmark), and low methoxy amidated pectin (0.20% LM-106 AS-YA). The activated PBC was pre-homogenized at 3500 psi, followed by upstream UHT homogenization at 70 °C, and then pasteurized at 99 °C for 2 minutes. Extrusion force of the samples was measured after refrigeration for 1 week using TA/XT-2 Texture Analyzer, TA-425 Spread Rig on three replicate samples. The results are shown in Table 25.

Table 25. Extrusion Force for Yoghurt White Mass

Example 17. Vanilla Preparation for Yoghurt

Vanilla preparations at 10%> soluble solids for use in yoghurt were prepared using the activated PBC having a coil overlap parameter of 3.09 that was expanded using a high shear mixer or homogenizer and compared to typical starch containing vanilla preparations. Formulations are shown in Table 26.

Table 26. Vanilla Preparations

The activated PBC was dispersed in water at ambient temperature and expanded either 1) in a high shear mixer at 7500 rpm for 10 minutes or 2) in a high shear mixer at 5000 rpm for 10 minutes followed by homogenization at 200/50 bar. The starch was dispersed into water at ambient temperature while stirring. Sucrose, tri-natrium citrate, calcium chloride solutions, and vanilla grains were added to the water/citrus fiber or water/starch concentrations while stirring. The mixture was then heated to 90 °C while stirring and held for 15 minutes. Potassium sorbate was added, and the mixture was adjusted to 100 weight percent by adding water. The vanilla preparation was filled into a container and placed on cold storage.

The expanded PBC provides a smooth and shiny appearance, whereas starch provides a dull appearance. The expanded PBC provides texture, mouthfeel and suspension similar to that of natural starch. Syneresis control was exhibited. The vanilla preparation was easy to stir into yoghurt white mass and provided a nice smooth yoghurt appearance, with no sandy mouthfeel. Example 18. Neutral Protein Drinks

Neutral protein drinks were made using the activated PBC of Sample 1A. A 1.5% activated PBC solution was prepared by using a Silverson at 8000 rpm for 20 minutes, then adjusting the pH to 6.6-6.7 by using 8% sodium bicarbonate. The neutral protein drinks underwent a UHT process by preheating at 65 °C for homogenization (200/20 bar), 141 °C for 5 seconds, and cool filled at 20-25 °C. The product viscosity was increased to provide stability improvement and enhanced mouthfeel. Formulations are shown in Table 27.

Table 27. NPD Formulations

Example 19. Fruit Flavored Drinks (no pulp/puree)

Fruit flavored drinks not containing juice were made using the activated PBC derived from citrus fruit having a coil overlap parameter of 3.09 (CF) and compared with other stabilizers - GENU® VIS pectin (GENU) and Keltrol® AP xanthan gum (KTL AP), both available from CP Kelco U.S., Inc. Formulations are shown in Table 28.

Table 28. FFD Formulations

The stabilizer or activated citrus fiber was dispersed into water at ambient temperature using high shear mixer at 5000 rpm for 10 minutes (GENU VIS sample was made with 80 °C. To prepare the fruit flavored drink, sucrose and tri-sodium-citrate were added to the stabilizers or expanded citrus fiber and the pH was adjusted to 3.6 using citric acid while stirring. The mixture was then heated to 85 °C in a 95 °C bath and held for 15 minutes, then homogenized at 200/50 bar, then cooled to 25-30 °C, and then filled into containers and placed in cold storage.

The trial use levels and measured pH and soluble solids are summarized in Table 29.

Table 29

The expanded citrus fiber provided higher viscosity and mouthfeel when compared to a product made with pectin and xanthan gum and the resulting fruit flavored drinks provided an opaque appearance resembling fruit pulp/puree inclusion.

Example 20. Fruit Flavored Drinks (with pulp/puree)

Fruit flavored drinks containing juice, pulp and puree were made using the activated PBC derived from citrus fruit having a coil overlap parameter of 3.09. Formulation for orange juice is shown in Table 30.

Table 30. Orange Juice Drink

Finished Drink Ingredients % Weight

Orange juice drink 96

Orange sacs 4

Total 100

The process for preparing the orange juice drink was as follows: 1) disperse activated citrus fiber in ambient temperature water using a Silverson rotor stator mixer at 5000 rpm for 5 minutes; 2) dry blend sugar and tri sodium citrate; add to citrus fiber solution while mixing with Silverson mixer; 3) add orange juice concentrate; continue mixing at 5000 rpm for 5 minutes; 4) adjust pH to 3.6 using citric acid solution; 5) adjust final solids to 11.0° Brix using sugar; 6) UHT process at 110 °C for 6 seconds with upstream homogenization at 200/50 bar (2900/730 psi) in 2 stages; 7) aseptically fill into pre- sterilized glass bottles containing orange sacs at 25-30 °C.

The activated citrus fiber expanded during mixing with the Silverson and during normal UHT process. The activated citrus fiber was useful across low pH ranges and able to suspend orange sacs from pH 2.8 - 4.0. The orange juice drink had enhanced mouthfeel at a lower dosage of activated citrus fiber as compared to using pectin.

A formulation for reduced puree mango drink using the activated citrus fiber is shown in Table 31.

Table 31. Mango Drink

The process for preparing the mango drink was as follows: 1) Disperse activated citrus fiber in ambient temperature water using a Silverson rotor stator mixer at 5000 rpm for 5 minutes; 2) dry blend sugar and ascorbic acid; add into the activated citrus fiber solution while mixing with Silverson mixer; 3) add mango puree concentrate and continue mixing at 5000 rpm for 5 minutes; 4) adjust pH to 3.4 using citric acid solution; 5) adjust final solids to 15o Brix using sugar; 6) add mango flavor and mix to incorporate; 7) UHT process at 110 °C for 6 seconds with upstream homogenization at 200/50 bar in 2 stages; 8) hot fill into PET bottles at 85-90 °C; and 9) cool bottles in a water bath to ambient temperature.

The activated citrus fiber expanded during normal UHT process, was able to compensate for mouthfeel reducing the mango puree from 15.5% to 10.5%, provided suspension of mango pulp and prevented sedimentation. The mango drink was stable through UHT heat treatment and subsequent hot filling.

Example 21. Ice Cream

Ice cream formulations were made using the activated PBC derived from citrus fruit having a coil overlap parameter of 2.74 and compared to a reference material of Palsgaard blend and Herbacel AQ Plus Citrus Fiber. The ice cream had a standard overrun of 80- 120% and a formulation are noted below in Table 32.

Table 32. Ice Cream Full Fat (10%) Formulations

*Palsgaard® Extrulce 255: Mono- and Di-glycerides, Guar gum, Locust bean gum and 2 types of antioxidants

The basemix was prepared using a high sear mixer (Silverson rotor stator mixer with Emulsor screens 1.5 mm) as follows: 1) mix all dry ingredients, 2) heat milk/glucose blend to 40 °C, 3) add dry mix to milk/glucose blend, using Silverson at 7500 rpm/5 min, 4) add cream and run 1 more minute at 5000 rpm, 5) heat to 75 °C and homogenize two stages 170/25 bar, 6) heat to 90 °C and hold for 5 minutes while stirring, 7) cool the ice cream mix overnight (ripening) before freezing. The freezing process - ice cream machine (Day+1) was as follows: 1) transfer ice cream base into freezer chamber or cylinder, 2) whip the mix while freezing to the desired temperature and % overrun (80-120%), 3) fill ice cream into containers, and 4) place immediately in a freezer according to standard conditions, evaluate base mix stability, measure pH and viscosity, 2) weight off 2kg base mix and fill into freezing chamber - start timer, 3) freeze according to desired test conditions and note temp, time and % OR, 4) fill ice cream into suitable cups for measurements/evaluation, and 5) place immediately the ice cream in a freezer (-18 °C) until evaluation. The performance of the various materials is noted below in Table 33.

Table 33. Ice Cream Performance

Activated citrus fiber may be used as a single stabilizer, replacing stabilizer blends, traditionally used in ice cream and provides stability and viscosity of ice cream mix, improves incorporation of air, reduces ice crystal growth, improves mouthfeel and syneresis/wheying off. In the data above, the Pals samples had stabilizers and emulsifiers whereas the PBC and H.AQ Plus samples did not. The use of emulsifiers at 0.1 to 0.3 % may reduce whipping time, enhance body and improve meltdown.

Example 22. Thicken Bouillon Concentrate

The activated pectin-containing biomass composition (PBC) of Example IB was evaluated for use as a bouillon concentrate (fond) thickener, such as would be used in the production of a sauce, gravy or marinade. Samples containing 1%, 2% and 4% activated pectin-containing biomass were compared to a sample with no viscosifier and a sample thickened with 2% or 4% modified starch (THERMTEX modified starch, Ingredion Incorporated, Bridgewater, NJ). 50 % dry powder mix (containing OSCAR Vegetable bouillon granulate and the viscosifier) and 50 % tap water, were mixed to disperse the components, and the dispersion was heated to the boiling point and maintained at boiling for 3 minutes. The boiled mixture then was transferred to an 800 mL beaker and allowed to cool to room temperature. The viscosity of each formulation was measured. For low viscosity samples, viscosity was measured using a Brookfield LVF viscometer with spindle 3 at 60 rpm for 30 sec. For high viscosity samples, viscosity was measured using a Brookfield RVT viscometer with spindle 6 at 50 rpm for 30 sec. The formulations and results are shown in Table 34.

Table 34. Bouillon Concentrate Formulations and Testing Data

Ready to taste bouillons were prepared using a dosage of 20 g bouillon concentrate and 480 g boiling water. When the samples containing 2% activated pectin-containing biomass composition and 4% THERMTEX modified starch were compared for flavor, an increase in flavor masking was observed for the modified starch sample. Accordingly, the activated pectin-containing biomass composition can be used to replace modified starch in such savory applications as bouillon concentrate, gravies, sauces, and soups.

Example 23. Soup

Soups were made using the activated PBC having a coil overlap parameter of 3.09. A formulation for cream of mushroom soup is shown in Table 35. Table 35. Cream of Mushroom Soup

The creme base had the following weight percent of ingredients: 72.8 water, 19 soybean oil, 3.2 Arcon® soy protein concentrate from ADM, 3.2 unsalted butter, 1.5 JOHA® KM 2 sodium phosphate blend from ICL, and 0.3 Datem emulsifier powder. All ingredients for the creme base were mixed together with moderate agitation, warmed to 40 °C to melt butter and emulsifier, and homogenized using APV Gaulin homogenizer sent to 145/30 bar first/second stage.

The procedure for making the creme of mushroom soup was as follows: 1) disperse activated citrus fiber in water and mix with Silverson rotor stator mixer for 1 minute @ 7000 rpm; 2) expand with 2 passes through APV Gaulin homogenizer @ 200 bar; 3) combine heavy cream, creme base and expanded citrus fiber; 4) while stirring with propeller mixer, mix in dry ingredients and fully disperse; 5) add the mushrooms and onions; and 6) fill into cans with 10 mm (3/8 inch) headspace, steam purge, seal and heat using retort sterilization process. A formulation for tomato soup is shown in Table 36.

Table 36. Tomato Soup

The procedure for making the tomato soup was as follows: 1) disperse activated citrus fiber in water and mix with Silverson rotor stator mixer for 1 minute @ 7000 rpm; 2) expand the activated citrus fiber with 2 passes through the APV Gaulin homogenizer @ 200 bar (3000 psi); 3) thoroughly mix water tomato paste and soybean oil; add expanded citrus fiber using propeller mixer; 4) blend sugar, salt, starch, spices and acids and add to the above concentration while mixing; 5) mix until all ingredients are fully dispersed; 6) add basil and parsley and mix; 7) fill into cans with 10 mm (3/8 inch) headspace, steam purge, seal and heat using retort sterilization process.

The soups had a smooth and slightly pulpy appearance. The texture did not thin much with heating and was short and not stringy. There was good stabilization of the emulsion even during heating, thus allowing for the use of the expanded citrus fiber during retorting. Further, the starch was reduced resulting in reduced calories.

Example 24. Granola or Protein Snack Bar

Snack bars were made using the activated PBC derived from citrus fruit having a coil overlap parameter of 2.74 in a formulation as follows in Table 37. The formulation was prepared to replace 20% oligofructose with activated citrus fiber and no added sugar. Table 37. Snack Bar Formulation

The expanded PBC was prepared using a Silverson mixer at 8000 rpm for 5 minutes. The snack bars were prepared by blending the dry ingredients except for the puffed rice, adding the wet ingredients (including expanded PBC, activated PBC and oil) to the bowl, mixing on a Hobart mixer at full power for 1 minute, adding puffed rice, continuing mixing by hand, flattening on baking paper and backing in oven at 170 °C for 25 minutes. The pectin-containing biomass composition provided nutritional benefits, supported a simple and clean label, glued the granola mass together during baking, replaced sugar or oligofructose for calorie reduction, and contributed structure and fiber enrichment. Example 25. Toothpaste

The ability of the activated pectin-containing biomass composition was shown to thicken a toothpaste formulation. Two formulations processed with different mixing speeds were evaluated. The formulations and mixing speeds are shown in Table 38.

Table 38. Formulations and Mixing Speed

In the first run, the activated pectin-containing biomass composition of Example 1 A was dispersed in the glycerol while stirring with a propeller stirrer at 1,400 rpm for 10 minutes. In the second run, the activated pectin-containing biomass composition of Example 1 A was dispersed in the glycerol while stirring with a propeller stirrer at 800 rpm for 10 minutes.

For both runs, the sodium chloride then was added with mixing, and mixing continued an additional 5 minutes. The mixture then was heated to 80°C for 30 minutes with mixing. The mixture then was transferred to a ROSS mixer pot (double planetary mixer, Charles Ross & Son Company, Hauppauge, NY) and the silica was added, and the mixture was mixed for 20 minutes at 100 rpm with vacuum.

The product of run number 1 was thick and pasty. The product of run number 2 had a squeezable toothpaste consistency and was able to form a nurdle that could retain its shape after being dispensed.

Example 26. Humectant for a Moisturizer

Formulations containing 1 wt% and 3 wt% activated pectin-containing biomass composition of Example 1A in glycerol were prepared and evaluated for use as a moisturizer. The activated pectin-containing biomass composition was dispersed in the glycerol while stirring with a propeller stirrer approx 600 rpm for 10 minutes. The viscosity then was measured using a Brookfield Viscosimeter DV2T at 25°C, 30 rpm for 1 minute (initial viscosity). The mixture then was transferred to a water bath and heated to 80°C, and maintained at 80°C for 30 minutes. The mixture then was transferred to a capped bottle and allowed to cool to room temperature overnight. The mixture was heated to 25°C and the viscosity at 25°C was measured with a Brookfield Viscosimeter DV2T at 30rpm for 1 minute. The results are shown in Table 39.

Table 39. Formulation Viscosities

The activated pectin-containing biomass composition at a usage level of 1 wt% was able to increase the viscosity of the glycerol by about 1.6 times after 24 hours, but the solution was separated into two phases. The activated pectin-containing biomass composition at a usage level of 3 wt% was able to increase the viscosity of the glycerol by about 5.9 times after 24 hours. Both formulations could be applied easily to the skin.

Example 27. Film Former

The ability of the activated pectin-containing biomass composition to form a film was evaluated. 3% activated pectin-containing biomass composition of Example 1A was dispersed in the glycerol while stirring with a Silverson high speed mixer at 7,400 rpm using an emulation screen 1mm- 1.5mm for 10 minutes. At the end of the mixing, the temperature of the mixture was 135°C. The mixture was very thick but spreadable. A portion was spread on a silicone sheet, and a portion was allowed to cool in a plastic weigh boat. After cooling down at room temperature overnight, the portion spread on the sheet formed a very strong film, while the mixture in the weigh boat became a very strong gel.

While various embodiments of the subject matter provided herein have been described, it should be understood that they have been presented by way of example only, and not limitation. Since modifications will be apparent to those of skill in this art, it is intended that this invention be limited only by the scope of the appended claims.

Claims

Claims:

1. A method for preparing an expanded pectin-containing biomass composition, the method comprising:

mixing an activated pectin-containing biomass composition with a fluid to form a mixture; and

subjecting the mixture to an extensional stress,

wherein:

a) the activated pectin-containing biomass composition has (i) a coil overlap parameter within the range of at or about 2 to at or about 4.5 when a starting biomass composition is citrus fruit; (ii) a coil overlap parameter 0.5 to at or about 2.0 when a starting pectin-containing biomass composition is from apple, Jerusalem artichoke or beet, or (iii) a coil overlap parameter at least about 300 percent greater than that of a coil overlap parameter of a starting pectin-containing biomass material; or

b) the activated pectin-containing biomass composition has an apparent viscosity from about 150 mPa*s to about 3500 mPa*s when measured in aqueous solution at a temperature of 25 °C and a pH of 4.0; or

c) the activated pectin-containing biomass composition comprises pectin in an amount from at or about 20 wt% to at or about 50 wt%, and cellulosic fiber in an amount from at or about 80 wt% to at or about 50 wt%; or

d) the activated pectin-containing biomass composition is substantially free of D- limonene; or

e) any combination of a), b), c) and d).

2. The method of claim 1, wherein the extensional stress is applied to the mixture by a propeller mixer, a rotor stator mixing device, a homogenizer or a combination thereof.

3. The method of claim 2, wherein the extensional stress is applied to the mixture by a rotor stator mixing device selected from among a Silverson mixer, a toothed-ring disperser, an annular-gap mill or a colloid mill or a combination thereof.

4. The method of claim 2, wherein the extensional stress is applied to the mixture by passing through a homogenizer selected from among a pressure homogenizer, a high pressure homogenizer, a microfiuidizer, a French press homogenizer, or an extensional homogenizer, or any combination thereof.

5. The method of claim 4, wherein the mixture is passed through the homogenizer at least 2 times.

6. The method of claim 4 or 5, wherein the high pressure homogenizer is operated at a pressure of at least 3,000 psi.

7. The method of any one of claims 1 to 6, wherein the fluid is aqueous or nonaqueous.

8. The method of any one of claims 1 to 7, wherein the fluid is at least a portion of a liquid component of a composition comprising the liquid component and one or more ingredients.

9. The method of claim 8, wherein:

the one or more ingredients of the composition are added to the mixture prior to subjecting the mixture to an extensional stress; or

the one or more ingredients of the composition are added to the mixture after subjecting the mixture to an extensional stress.

10. An expanded pectin-containing bio mass composition produced by the method of any one of claims 1 to 9.

11. The expanded pectin-containing biomass composition of claim 10 that exhibits a synergistic interaction with a protein or a hydrocolloid or both.

12. The expanded pectin-containing biomass composition of claim 11, wherein: the protein is a soy protein, egg white, sodium caseinate, milk protein, or a whey protein; or

the hydrocolloid is a starch, a xanthan gum, a pectin or a combination thereof.

13. The expanded pectin-containing biomass composition of any one of claims 10 to 12 that has a viscosity at 0.25% in water of at least at or about 500 mPa*s at 3 rpm on a Brookfield viscometer.

14. A composition, comprising:

from at or about 0.01 wt% to at or about 1 wt% of the expanded pectin-containing biomass composition of any one of claims 10 to 13; or from at or about 0.01 wt% to at or about 5 wt% of an activated pectin-containing biomass composition having a coil overlap parameter of 2 or greater.

15. The composition of claim 14 that is a food, industrial, oilfield, pharmaceutical, nutraceutical, dermato logical, cosmetic, household care, or personal care product.

16. The composition of claim 15 that is a yogurt fruit preparation, a salad dressing, a preserve, a jam, a jelly, a low sugar or no-sugar added fruit spread, a fruit pie filling, a fruit concentrate for ice cream manufacturing, an ice cream topping, a fruit leather, a sorbet, a dairy dessert, an ice cream, an ice milk, a non-dairy dessert, a water ice, a pudding, a custard, a mayonnaise, a low-fat or non-fat mayonnaise, a margarine, a low- fat spread, a sour cream, a low fat or non-fat sour cream, a peanut butter, a nut spread, a chocolate spread, an extruded snack, a soup, a sauce, a gravy, a marinade, a carbonated beverage, an energy drink, a fruit juice, a vegetable juice, a cocoa-based beverage, a chocolate syrup, a dairy beverage, a chocolate milk, a beverage concentrate, an acidified protein drink, a drinkable yogurt, a yogurt, a whipped yogurt, a cheese spread, a processed cheese, a batter, a coating, a whipped topping, a liquid fond concentrate, a bouillon, a whipped topping, a marshmallow product, a confection product, a whipped confection product, a candy, a toothpaste, a dental rinse, a ketchup, a barbeque sauce, a dysphagia product, a breakfast cereal, a baked good, a pastry, a cake, a patisserie, a cookie, a pie crust, a bread, a cracker, a thermostable filling having a low or ultra-low water activity, a dairy product, a meat additive, a meat extender, a paper, a paper coating, a nonwoven, a specialty laid sheet, a dielectric sheet, a battery separator, a capacitor separator, a fracturing fluid, a drilling mud, a weighted or inhibited fluid for oilfield applications, a gravel packing composition, a cementing formulation, a spacer fluid, a pore former in a ceramic or catalyst composition, a flocculation medium, a fining agent, a filter medium, a tub or tile cleaner, a hard surface cleaner, a dish detergent, a floor cleaner, a carpet cleaner, a sanitizer, a wood and furniture polish, a toilet bowl cleaner, an antifog agent, a drain cleaner, a scale remover, a paint, a paint remover, a stain, a stain remover, a dye, a printing ink, a nutraceutical, a pharmaceutical elixir, a suspension, a syrup, a tablet binder, a tablet disintegrant, a pet product, an animal feed product, a shampoo, a conditioner, a cream, a styling gel, a sun screen, a hand or body lotion, a fabric detergent, a high surfactant laundry detergent, a fabric conditioner, a wax suspension, a weed control composition, or an agricultural emulsion.

17. The composition of claim 15 or 16 that is a food product, and the expanded pectin-containing biomass composition or the activated pectin-containing biomass composition replaces at least a portion of a fat or a carbohydrate or both in the food product, resulting in a reduced calorie content or a reduced fat content or both.

18. The composition of any one of claims 15 to 17 that is a food product having an improved texture, an improved mouthfeel or an improved flavor release compared to a comparable food product in which the expanded pectin-containing biomass composition or activated pectin-containing biomass composition is not present.

19. The composition of any one of claims 15 to 18, wherein the food product is an emulsion, a foam, a batter or a dough.

20. The composition of any one of claims 14 to 19, wherein the expanded pectin- containing biomass composition or activated pectin-containing biomass composition: a) suspends particulates in the composition; or

b) minimizes coalescence of fat globules in the composition; or

c) minimizes coalescence of air bubbles in the composition; or

d) any combination of a), b) and c).

21. The composition of claim 20 that is a pharmaceutical, cosmetic,

dermatological or personal care product, and further comprises an active ingredient.

22. A method for modifying a rheological property of a composition, comprising: adding to the composition an amount of the expanded pectin-containing biomass composition of any one of claims 10 to 13 or an activated pectin-containing biomass composition having a coil overlap parameter of 2 or greater sufficient to increase the viscosity, or to modulate the yield stress of the composition.

23. The method of claim 22 where the composition is a food, industrial, pharmaceutical, nutraceutical, cosmetic, oilfield, household care, or personal care product.

24. A method for altering a physical or processing property of a composition, comprising:

adding to the composition an amount of the expanded pectin-containing biomass composition of any one of claims 10 to 12, or an activated pectin-containing biomass composition having a coil overlap parameter of 2 or greater, sufficient to alter a physical property or processing property of the composition.

25. The method of claim 24, wherein the composition is a food, industrial, pharmaceutical, nutraceutical, dermatological, cosmetic, oilfield, household care, or personal care product.

26. The method of claim 24 or 25, further comprising exposing the composition to an extensional stress after the expanded pectin-containing biomass composition or the activated pectin-containing biomass composition has a coil overlap parameter of 2 or greater is added to the components.

27. The method of claim 26, wherein the extensional stress is applied by a propeller mixer, a rotor stator mixing device, a homogenizer or a combination thereof.

28. The method of claim 27, wherein the extensional stress is applied by a rotor stator mixing device selected from among a Silverson mixer, a toothed-ring disperser, an annular-gap mill or a colloid mill or a combination thereof.

29. The method of claim 27, wherein the extensional stress is applied by passing through a homogenizer selected from among a pressure homogenizer, a high pressure homogenizer, a microfluidizer, a French press homogenizer, or an extensional

homogenizer, or any combination thereof.

30. The method of claim 29, wherein the composition is passed through the homogenizer at least 2 times.

31. The method of claim 29 or 30, wherein the high pressure homogenizer is operated at a pressure of at least 3,000 psi.

32. The method of any one of claims 24 to 31 , wherein the composition is a yogurt fruit preparation, a salad dressing, a preserve, a jam, a jelly, a low sugar or no-sugar added fruit spread, a fruit pie filling, a fruit concentrate for ice cream manufacturing, an ice cream topping, a fruit leather, a sorbet, a dairy dessert, an ice cream, an ice milk, a non- dairy dessert, a water ice, a pudding, a custard, a mayonnaise, a low- fat or non-fat mayonnaise, a margarine, a low- fat spread, a sour cream, a low fat or non-fat sour cream, a peanut butter, a nut spread, a chocolate spread, an extruded snack, a soup, a sauce, a gravy, a marinade, a carbonated beverage, an energy drink, a fruit juice, a vegetable juice, a cocoa-based beverage, a chocolate syrup, a dairy beverage, a chocolate milk, a beverage concentrate, an acidified protein drink, a drinkable yogurt, a yogurt, a whipped yogurt, a cheese spread, a processed cheese, a batter, a coating, a whipped topping, a liquid fond concentrate, a bouillon, a whipped topping, a marshmallow product, a confection product, a whipped confection product, a candy, a toothpaste, a dental rinse, a ketchup, a barbeque sauce, a dysphagia product, a breakfast cereal, a baked good, a pastry, a cake, a patisserie, a cookie, a pie crust, a bread, a cracker, a thermostable filling having a low or ultra-low water activity, a dairy product, a meat additive, a meat extender, a paper, a paper coating, a nonwoven, a specialty laid sheet, a dielectric sheet, a battery separator, a capacitor separator, a fracturing fluid, a drilling mud, a weighted or inhibited fluid for oilfield applications, a gravel packing composition, a cementing formulation, a spacer fluid, pore former in a ceramic or catalyst composition, a flocculation medium, a fining agent, a filter medium, a tub or tile cleaner, a hard surface cleaner, a dish detergent, a floor cleaner, a carpet cleaner, a sanitizer, a wood and furniture polish, a toilet bowl cleaner, an antifog agent, a drain cleaner, a scale remover, a paint, a paint remover, a stain, a stain remover, a dye, a printing ink, a nutraceutical, a pharmaceutical elixir, a suspension, a syrup, a tablet binder, a tablet disintegrant, a pet product, an animal feed product, a shampoo, a conditioner, a cream, a styling gel, a sun screen, a hand or body lotion, a fabric detergent, a high surfactant laundry detergent, a fabric conditioner, a wax suspension, a weed control composition, or an agricultural emulsion.

33. A method for reducing the caloric content of a food product, comprising replacing one or more of a fat, a sugar, or a starch or a portion thereof by adding an amount of the expanded pectin-containing biomass composition of any one of claims 10 to 13, or an activated pectin-containing biomass composition having a coil overlap parameter of 2 or greater, sufficient to yield a food product having commercially acceptable physical and processing characteristics.

34. An expanded pectin-containing biomass composition product, as disclosed herein.

35. A method for preparing an expanded pectin-containing biomass composition product, as disclosed herein.

36. Use of the expanded pectin-containing biomass composition product of any one of claims 10 to 13, or an activated pectin-containing biomass composition having a coil overlap parameter of 2 or greater, to modify a rheological property of a composition.

37. Use of the expanded pectin-containing biomass composition product of any one of claims 10 to 13, or an activated pectin-containing biomass composition having a coil overlap parameter of 2 or greater to alter a physical property of a composition.

38. Use of the expanded pectin-containing biomass composition product of any one of claims 10 to 13, or an activated pectin-containing biomass composition having a coil overlap parameter of 2 or greater, to alter a processing property of a composition.

39. Use of the expanded pectin-containing biomass composition product of any one of claims 10 to 13, or an activated pectin-containing biomass composition having a coil overlap parameter of 2 or greater, to reduce the caloric content of a food product.