EP4688942A1 - A composition comprising a pectin and water - Google Patents

A composition comprising a pectin and water

Info

Publication number
EP4688942A1
EP4688942A1 EP24721831.6A EP24721831A EP4688942A1 EP 4688942 A1 EP4688942 A1 EP 4688942A1 EP 24721831 A EP24721831 A EP 24721831A EP 4688942 A1 EP4688942 A1 EP 4688942A1
Authority
EP
European Patent Office
Prior art keywords
pectin
weight
composition
degree
amidated
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
EP24721831.6A
Other languages
German (de)
French (fr)
Inventor
Gueba AGODA-TANDJAWA
Didier Marcel Norbert BEKAERT
Clémence Anne Geneviève Marie GALLERY DES GRANGES
Lorenzo GITTO
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Cargill Inc
Original Assignee
Cargill Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Cargill Inc filed Critical Cargill Inc
Publication of EP4688942A1 publication Critical patent/EP4688942A1/en
Pending legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L5/00Compositions of polysaccharides or of their derivatives not provided for in groups C08L1/00 or C08L3/00
    • C08L5/06Pectin; Derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/0003General processes for their isolation or fractionation, e.g. purification or extraction from biomass
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/0006Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
    • C08B37/0045Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid alpha-D-Galacturonans, e.g. methyl ester of (alpha-1,4)-linked D-galacturonic acid units, i.e. pectin, or hydrolysis product of methyl ester of alpha-1,4-linked D-galacturonic acid units, i.e. pectinic acid; Derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/02Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
    • C08J3/03Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
    • C08J3/075Macromolecular gels
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L29/00Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/20Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/206Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
    • A23L29/231Pectin; Derivatives thereof

Definitions

  • the present invention relates to a composition comprising a pectin and water, and a method of making the composition.
  • the composition has properties useful to the food and/or beverage industry.
  • Pectin is found naturally in plant cell walls. Although pectin can be extracted from a large number of plants or fruits, the main industrial or conventional sources include citrus peel and apple pomace. The main use of pectin is as a gelling agent, thickening agent, viscosifying agent and/or as a stabiliser in food. As a result, pectin is commonly used in jams, jellies, acid milk beverages and dessert bases as a food additive. Pectin can also be used as dietary fibers and as an effective food emulsifier. Pectin also has potential uses in other fields such as medicine as a carrier for controlled drugs or bioactive release and in many other nonfood applications.
  • Pectin is a polysaccharide comprising a chain of galacturonic acid units which are linked by a- 1,4 glycosidic bonds.
  • the galacturonic acid chain may partly be esterified as methyl esters.
  • the galacturonic acid chain is the backbone of pectin, other chemicals such as acetyl and methyl ester groups can be incorporated into the chain. These groups can be important for distinguishing between different pectin types.
  • Pectin can be split into two categories by its degree of methylation, which is the percentage of carboxyl groups which have undergone esterification with methanol. The degree of methylation is of great importance for the use of pectins as gelling agents and depending on the degree of methylation, the pectin is classified as either a high methoxyl pectin (HM pectin) or a low methoxyl pectin (LM pectin). If more than 50 percent of the carboxyl groups are methylated then the pectin is a HM pectin, and if less than that degree of methylation has occurred then the pectin is a LM pectin.
  • HM pectin high methoxyl pectin
  • LM pectin low methoxyl pectin
  • HM pectin is the most commonly used pectin and can be split into two categories: rapid set HM pectin and slow set HM pectin. Rapid set pectin will set faster and at a higher temperature than slow set pectin, and thus is preferable in the production of food and/or beverage products which typically require a certain mouthfeel or the suspension of various particulate matter such as whole or portioned fruits, nuts and the like. Slow set pectin is preferable for food and/or beverage products which do not require the presence of suspended particulate matter. HM pectins can form gels with sugar and acid, forming what is known in the art as low water activity gels or sugar acid pectin gels.
  • Slow set pectin can take from 1 to 2 days to set into a gel.
  • These gels have a 3-dimensional network of pectin molecules in which a solvent (usually water), optionally with the co-solutes of sugar and acid are immobilised resulting in a system that can resist deformation.
  • LM pectins differ from HM pectins in that the LM pectins only require the presence of a divalent cation to initiate the reaction that causes the pectin to set into a gel.
  • the most commonly used divalent cation is calcium.
  • the gel forming ability of LM pectins increases with a decreasing degree of methylation.
  • LM pectins have been amidated to form LM amidated pectin.
  • LM ami dated pectin is a modified form of LM pectin in which some of the galacturonic acid units are converted by ammonia into carboxylic amides.
  • a HM pectin needs to be first extracted from its natural source.
  • the HM pectin is converted into LM pectin, which undergoes amidation to form the LM amidated pectin.
  • the conversion of the HM pectin into LM amidated pectin follows the reaction scheme:
  • a LM amidated pectin is advantageous compared to non-amidated LM pectins because the LM amidated pectin can enlarge the calcium sensitivity tolerance of LM pectins and therefore permit gelation over a wider range of calcium concentrations unlike non-amidated LM pectins.
  • amidated pectins are typically thermo-reversible: LM amidated pectins can be heated to form a liquid and after cooling solidify again, whereas conventional pectin-gels will remain in liquid form after heating and cooling.
  • LM amidated pectins can promote the stabilisation of junction zones of pectin gel network structures through additional hydrogen bond formation with the amide groups. Further advantageously, LM amidated pectins display good gelling properties under low-sugar conditions.
  • LM amidated pectins are regularly used in the food and/or drink industry. There is thus a continuous need for improved pectins and compositions comprising the pectins, which can be used in the food and/or beverage industry. In particular, there is a continuous need for improved LM amidated pectins and compositions comprising the LM amidated pectins, which can be used in the food and/or beverage industry.
  • the present invention relates to a composition comprising a pectin and water, and a method of making the composition.
  • the composition has properties useful to the food and/or beverage industry.
  • DE degree of esterification
  • DA degree of amidation
  • DE degree of esterification
  • DA degree of amidation
  • DE degree of esterification
  • DA degree of amidation
  • Tg temperature of gelation
  • a pectin having: a degree of esterification (DE) of from 15 to 45 %, or from, 18 to 40 %, or, from 20 to 35 %. or, from 23 to 31 %, or 23.3 to 31 %. a degree of amidation (DA) of from 5 to 30 %, or, from 12 to 25 %, or, from 15 to 23 %, or, from 16 to 22. 1 ; and, a ratio of a degree of esterification (DE) to a degree of amidation (DA) of from 0.75 to 3.0, or, from 0.85 to 2.5, or. from 0.95 to 2.0. or, from 1.05 to 1.94.
  • DE degree of esterification
  • DA degree of amidation
  • a composition having a critical gelling concentration (Co) comprising: a pectin; and, water; and wherein the critical gelling concentration (Co) is from 0.01 to 0.2 weight %.
  • composition of clause 13, wherein the critical gelling concentration (Co) is from 0.02 to 0.17 weight %, or, from 0.025 to 0.15 weight %, or, from 0.04 to 0.13 weight %, or, from 0.05 to 0. 12 weight %.
  • composition of clause 13 or clause 14, wherein the pectin has a ratio of a degree of esterification (DE) to a degree of amidation (DA) of from 0.75 to 3.0, or, from 0.85 to 2.5, or, from 0.95 to 2.0, or. from 1.05 to 1.94.
  • DE degree of esterification
  • DA degree of amidation
  • the critical gelling concentration (Co) is 0.12 weight %: optionally, wherein the pectin has a ratio of a degree of esterification (DE) to a degree of amidation (DA) of 1.94.
  • a composition having a temperature of gelation (Tg) and a critical gelling concentration (Co) comprising: a pectin; and, water; wherein when the pectin concentration in the water increases from 0.8 weight % to 1.4 weight % relative to the total weight of the composition, the temperature of gelation (Tg) varies by from 0.5 to 2.5 °C; and wherein the critical gelling concentration (Co) is from 0.01 to 0.2 weight %.
  • DE degree of esterification
  • DA degree of amidation
  • DE degree of esterification
  • DA degree of amidation
  • Tg temperature of gelation
  • Co critical gelling concentration
  • sugar optionally, wherein the sugar is any one of sucrose, dextrose, lactose, maltose, glucose and/or galactose; optionally, wherein the sugar is present at from 20 to 60 weight %, or, from 30 to 50 weight %, or, from 35 to 45 weight %, or at 40 weight % relative to the total weight of the composition.
  • a pectin having: a degree of esterification (DE) of from 15 to 45 %; a degree of amidation (DA) of from 5 to 30 %; and a ratio of the degree of esterification (DE) to the degree of amidation (DA) of from 0.5 to
  • the pectin of clause 33 having a galacturonic acid content (GalA) of from 75 % or less, or, from 70 % or less, or, from 65 % or less, or, from 60 % or less, or. from 50 to 75 %. or, from 55 to 65 %. or, from 57 to 61 %. or, 59.0 %.
  • GalA galacturonic acid content
  • the degree of esterification (DE) to the degree of amidation (DA) is from 0.75 to 3.0, or, from 0.85 to 2.5, or. from 0.95 to 2.0. or, from 1.05 to 1.94.
  • the ratio of the degree of esterification (DE) to the degree of amidation (DA) is from 0.5 to 1.5, or, from 0.75 to 1.25, or, from 0.9 to 1.1, or. 1.05; wherein the pectin has a galacturonic acid content (GalA) of from galacturonic acid content (GalA) of from 85 % or greater, or, from 90 % or greater, or, from 85 % to 95 %, or, from 88 to 94 %, or, 93.0 %.
  • GalA galacturonic acid content
  • pectin of any one of clauses 33 to 43 wherein the pectin is a low methoxyl (LM) amidated pectin, optionally wherein the low methoxyl amidated pectin has a degree of methylation of below 50 %.
  • LM low methoxyl
  • a method of making a pectin according to any one of clauses 33 to 44 comprising the following steps: obtaining a high methoxyl (HM) pectin in aqueous form from a natural source; dry ing the high methoxyl (HM) pectin aqueous form to form a dry high methoxyl (HM) pectin, wherein the dry high methoxyl (HM) pectin has a moisture content of 10 weight % of the total weight of the dry 7 high methoxyl (HM) pectin; placing the dry' high methoxyl (HM) pectin in a suspension comprising alcohol and ammonia to form an amidated low methoxyl (LM) pectin; and, dry ing the amidated low methoxyl (LM) pectin to form a pectin; optionally, the method further comprising any one or more of the following steps: clarifying the high methoxyl (HM) pectin in aqueous form from
  • a composition comprising: a pectin; and, water; wherein the pectin is the pectin of any one of clauses 33 to 44; optionally, wherein the composition further comprises sugar.
  • the sugar is any' one of sucrose, dextrose, lactose, maltose, glucose and/or galactose; optionally, wherein the sugar is present at from 20 to 60 weight %. or, from 30 to 50 weight %, or, from 35 to 45 weight %, or, at 40 weight % of the total weight of the composition.
  • composition according to clause 47 Use of the composition according to clause 47, in a food and/or beverage product; optionally, wherein the food and/or beverage product is a dairy' product.
  • a method of making the composition of clause 47 comprising: providing a pectin; combining the pectin with water to form a composition; wherein the pectin is the pectin of any one of clauses 33 to 44; optionally, wherein the composition comprises the pectin at a concentration of from 0.001 to 10 weight % relative to the total amount of pectin and water, or, from 0.01 to 7.5 weight % relative to the total amount of pectin and water, or, from 0.
  • FIG. 1 is a flow diagram of a method for producing the pectin according to the present invention from dry HM pectin.
  • FIG. 2 is a plot of storage modulus (G’) and loss modulus (G”) for a composition comprising pectin and water according to the present invention (the composition analysed is Composition 1).
  • FIG. 3 is a plot of storage modulus (G’) versus concentration (C) for a composition comprising pectin and water according to the present invention (the composition analysed is Composition 1).
  • “Amidation” refers to the modification of a pectin to include at least one amide group (-NH2).
  • “Critical gelling concentration” refers to the lowest concentration of a substance in a solvent, at which the substance is able to form a gel.
  • a typical example is a composition comprising a pectin (i.e., the substance) in water (i.e., the solvent) with or without an additive (e.g., but not limited to sugars as defined herein below).
  • the critical gelling concentration is dependent on molecular characteristics (such as, but not limited to, the degree of esterification (DE) and/or the degree of amidation (DA)) and environmental conditions (such as, but not limited to, the nature of the solvent, the ionic strength, the type of salts present and pH).
  • composition refers to a mixture of at least two components.
  • the mixture can be a solution, a suspension, or a dispersion.
  • “Degree of amidation” refers to the percentage of carboxyl groups that are amides. Theoretically, the degree of amide groups can range from 0 to 100 %. Preferably, the degree of amidation for a pectin is from 5 to 30 %. The degree of amidation can be measured by titration, an example of such method being given in EP 1517925. the disclosure of which is hereby incorporated by reference in its entirety.
  • Degree of esterification refers to the percentage of carboxyl groups that have undergone esterification. Theoretically, the degree of esterification can range from 0 to 100 %. The degree of esterification is also referred in the art as degree of methyl-esterification or degree of methylation (DM). The degree of esterification can be measured by titration, an example of such method being given in EP1294920 and EPl 171473, the disclosures of which are hereby incorporated by reference in their entirety.
  • “Degree of methylation” refers to the percentage of carboxyl groups esterified with methanol. If more than fifty percent of the carboxyl groups are methylated the pectin is called high methoxyl pectins (HM), and if less than that degree of methylation has occurred then the pectin is called low methoxyl pectins (LM).
  • HM high methoxyl pectins
  • LM low methoxyl pectins
  • High methoxyl pectin or “HM pectin” refers to a pectin extracted from the peels of citrus fruit, wherein a degree of the original carboxyl groups present in the pectin have undergone esterification with methanol. High methoxyl pectins have a degree of methylation of above 50 %.
  • Low methoxyl pectin or “LM pectin” refers to a pectin extracted from the peels of citrus fruit, wherein a degree of the original carboxyl groups present in the pectin have undergone esterification with methanol. Low methoxyl pectins have a degree of methylation of below 50 %.
  • homogeneous refers to a substance with a uniform composition throughout.
  • a homogeneous substance does not present gradients of a certain property (e.g., concentration) larger than 1 weight % of the calculated property.
  • the composition may comprise a pectin, wherein the pectin is homogeneous (i.e., the composition comprises only one type of pectin).
  • pectin is herein understood that the pectin used in accordance with the invention is obtained from a single source of pectin and has a certain degree of amidation and a certain degree of esterification.
  • “Low methoxyl amidated pectin” or “LM amidated pectin” or “LMA pectin” refers to a modified form of LM pectin in which some or at least some of the methoxyl groups are converted by ammonia into carboxylic amides. Preferably, LM amidated pectins have a degree of amidation of from 5 and 30 %.
  • “Mix” or “mixture” refers to a substance containing two or more different components, whereas the term “mixed” refers to a method step wherein a mix or mixture is formed.
  • Pectin refers to an anionic water-soluble plant cell wall polysaccharide comprising a chain of galacturonic acid units which are linked by a-1,4 glycosidic bonds.
  • the galacturonic acid chain is partly esterified, i.e.. the galacturonic chain contains methyl ester groups.
  • Other chemicals such as acetyl can be incorporated into the galacturonic acid chain and can be important for distinguishing between different pectin types.
  • Pectin gel refers to a sample containing a three-dimensional (3-D) network of pectin molecules.
  • a pectin gel is the result of the association of long stretches of pectin polymer chain into conformationally ordered junction zones that are stabilised by arrays of noncovalent interactions.
  • Pectin gels possess both the viscous properties of liquids and the elastic properties of solids, i.e., they are viscoelastic materials.
  • Pectin gels have been known to the skilled person for decades, e.g. from M.A.V. Axelos et al.
  • Temporal of gelation refers to the temperature at which a material undergoes reverse thermal gelation, i.e., the temperature below which the material is soluble in water and above which the material undergoes phase transition to increase in viscosity or to form a serni-solid gel.
  • gelation temperature refers to the temperature at which a solution containing pectin transitions from a liquid state to a gel.
  • compositions according to the presently described invention have various desirable properties, which make these compositions useful for utilisation in various food and beverage products.
  • composition Temperature of gelation [00040]
  • the composition comprises a pectin and water.
  • the pectin is present in the composition in an amount of from 0.001 to 10 weight % relative to the total amount of pectin and water, preferably from 0.01 to 7.5 weight % relative to the total amount of pectin and water, more preferably from 0. 1 to 5 weight % relative to the total amount of pectin and water, even more preferably from 0.2 to 3 weight % relative to the total amount of pectin and water, even more preferably from 0.3 to 2.5 weight % relative to the total amount of pectin and water, most preferably from 0.4 to 2 weight % relative to the total amount of pectin and water.
  • the composition has a temperature of gelation (Tg), wherein when the concentration of the pectin relative to the total amount of pectin and water is increased from 0.8 weight % to 1.4 weight %, the temperature of gelation (Tg) varies by from 0.5 to 2.5 °C, preferably from 0.5 to 2.0 °C. more preferably from 0.75 to 1.5 °C, even more preferably from 1.0 to 1.3 °C, most preferably from 1.03 to 1.27 °C.
  • the concentration of the pectin in the water is increased from 0.8 weight % to 1.4 weight % relative to the total amount of pectin and water
  • the temperature of gelation (Tg) varies by from 1.03 to 1.27°C.
  • the pectin in the composition preferably has a degree of esterification (DE) of from 15 to 45 %, more preferably from 18 to 40 %, even more preferably from 20 to 35 %, even more preferably from 23 to 31 %, most preferably from 23.3 to 31.0 %.
  • DE degree of esterification
  • the pectin in the composition has a degree of amidation (DA) of from 5 to 30 %, more preferably from 12 to 25 %, even more preferably from 15 to 23 %, most preferably from 16.0 to 22.1 %.
  • DA degree of amidation
  • the pectin in the composition may have a ratio of a degree of esterification (DE) to a degree of amidation (DA) of from 0.75 to 3.0, preferably from 0.85 to 2.5, more preferably from 0.95 to 2.0, most preferably from 1.05 to 1.94.
  • DE degree of esterification
  • DA degree of amidation
  • the pectin in the composition has a degree of esterification (DE) of from 15 to 45 %, more preferably from 18 to 40 %, even more preferably from 20 to 35 %, even more preferably from 23 to 31 %, most preferably from 23.3 to 31.0 %; a degree of amidation (DA) of from 5 to 30 %, more preferably from 12 to 25 %, even more preferably from 15 to 23 %. most preferably from 16.0 to 22. 1 %, and. a ratio of a degree of esterification (DE) to a degree of amidation (DA) of from 0.75 to 3.0, preferably from 0.85 to 2.5, more preferably from 0.95 to 2.0, most preferably from 1.05 to 1.94.
  • DE degree of esterification
  • DA degree of amidation
  • the pectin in the composition has a degree of esterification (DE) of from 23.3 to 31 %, a degree of amidation (DA) of from 16.0 to 22. 1 %, and. a ratio of a degree of esterification (DE) to a degree of amidation (DA) of from 1.05 to 1.94.
  • DE degree of esterification
  • DA degree of amidation
  • DA degree of amidation
  • the pectin may be sourced from any one of apples, apple pomace, citrus fruits, citrus peel, lemons, mandarin oranges, grapefruit, sweet orange, pomelo, clementines, limes, kumquat, bitter oranges, blood oranges, satsumas, yuzus. tangelos, or, any combinations thereof.
  • the composition may comprise apple pectin, for example pectin extracted from apple pomace.
  • the composition may comprise apple pectin and water, and when the pectin concentration in the water is increased from 0.8 weight % to 1.4 weight % relative to the total amount of pectin and water, the temperature of gelation is 1.27°C.
  • said pectin also has a ratio of a degree of esterification (DE) to a degree of amidation (DA) of from 1.9 to 2.0, preferably, 1.94.
  • the entire amount of pectin present in the composition is apple pectin.
  • the composition may comprise citrus pectin, for example pectin extracted from citrus fruits, e.g., citrus peel.
  • the composition may comprise citrus pectin and water, and when the pectin concentration in the water is increased from 0.8 weight % to 1.4 weight % relative to the total amount of pectin and water, the temperature of gelation is 1.03 °C.
  • the pectin also has a ratio of a degree of esterification (DE) to a degree of amidation (DA) of from 1.00 to 1.10, preferably 1.05.
  • the entire amount of pectin present in the composition is citrus pectin.
  • the degree of esterification and the degree of amidation may be measured by titration techniques.
  • the pectin in the composition may be homogeneous.
  • the composition comprises pectin and water, wherein the pectin is preferably extracted from a single pectin source, said pectin source being chosen from the group consisting of apples, apple pomace, citrus fruits, citrus peel, lemons, mandarin oranges, grapefruit, sweet orange, pomelo, clementines, limes, kumquat, bitter oranges, blood oranges, satsumas, yuzus, tangelos, or, any combinations thereof.
  • the composition consists of a pectin and water, preferably, wherein the pectin is homogeneously distributed inside the water.
  • the pectin in the composition may be amidated.
  • the pectin in the composition may be a LM amidated pectin.
  • the composition may comprise sugar.
  • the sugar may be, but is not necessarily limited to, sucrose, dextrose, lactose, maltose, glucose and/or galactose.
  • the sugar is sucrose.
  • the composition comprises the sugar at from 20 to 60 weight %, more preferably from 30 to 50 weight %. even more preferably from 35 to 45 weight %, most preferably at 40 weight % of the total weight of the composition.
  • composition may additionally comprise a gel-promoting medium and/or a buffer.
  • the gel-promoting medium comprises citric acid monohydrate, tri-sodium citrate dihydrate, sodium benzoate, calcium chloride dihydrate and water.
  • the citric acid monohydrate is present at from 300 to 350 g, more preferably at from 320 to 330 g, most preferably at 325.598 g.
  • the trisodium citrate dihydrate is present at from 150 to 200 g, more preferably from 160 to 170 g, most preferably at 167.493 g.
  • the sodium benzoate is present at from 0.5 to 10 g, more preferably from 3 to 7 g, most preferably at 5 g.
  • the calcium chloride dihydrate is present at from 0.5 to 10 g, more preferably from 4 to 8 g, most preferably at 6.2 g.
  • the distilled water is present at from 4000 to 5000 g, more preferably, at from 4400 to 4600 g, most preferably at 4495.709 g.
  • the citric acid monohydrate is present at 325.598 g
  • the tri-sodium citrate dihydrate is present at 167.493 g
  • the sodium benzoate is present at 5 g
  • the calcium chloride dihydrate is present at 6.2 g
  • the distilled water is present at 4495.709 g.
  • the buffer comprises sodium citrate and water.
  • the buffer contains sodium citrate so that the pH of the buffer is from 3 to 4, more preferably from 3.2 to 3.6, most preferably 3.4.
  • the composition has a temperature of gelation (Tg) wherein when the concentration of the pectin relative to the total amount of pectin and water is increased from 0.8 weight % to 1 .4 weight %, the temperature of gelation (Tg) varies by from 0.5 to 2.5°C; and wherein the composition further comprises a gel-promoting medium and a buffer; wherein the gel-promoting medium comprises citric acid monohydrate, tri-sodium citrate dihydrate, sodium benzoate, calcium chloride dihydrate and water; and wherein the buffer comprises sodium citrate and water.
  • Tg temperature of gelation
  • composition Critical gelling concentration
  • the composition comprises a pectin and water.
  • the pectin is present in the composition in an amount of from 0.001 to 10 weight % relative to the total amount of pectin and water, preferably from 0.01 to 7.5 weight % relative to the total amount of pectin and water, more preferably from 0. 1 to 5 weight % relative to the total amount of pectin and water, even more preferably from 0.2 to 3 weight % relative to the total amount of pectin and water, even more preferably from 0.3 to 2.5 weight % relative to the total amount of pectin and water, most preferably from 0.4 to 2 weight % relative to the total amount of pectin and water.
  • the composition has a critical gelling concentration (Co) of from 0.01 to 0.2 weight %, preferably from 0.02 to 0.17 weight %, more preferably from 0.025 to 0.15 weight %, even more preferably from 0.04 to 0. 13 weight %, most preferably from 0.05 to 0. 12 weight %.
  • Co critical gelling concentration
  • the pectin in the composition preferably has a degree of esterification (DE) of from 15 to 45 %, more preferably from 18 to 40 %, even more preferably from 20 to 35 %, even more preferably from 23 to 31 %. most preferably from 23.3 to 31.0 %.
  • the pectin in the composition has a degree of amidation (DA) of from 5 to 30 %, more preferably from 12 to 25 %. even more preferably from 15 to 23 %, most preferably from 16.0 to 22.1 %.
  • the pectin in the composition may have a ratio of a degree of esterification (DE) to a degree of amidation (DA) of from 0.75 to 3.0, preferably from 0.85 to 2.5, more preferably from 0.95 to 2.0, even most preferably from 1.05 to 1.94.
  • DE degree of esterification
  • DA degree of amidation
  • the pectin in the composition has a degree of esterification (DE) of from 15 to 45 %, more preferably from 18 to 40 %, even more preferably from 20 to 35 %, even more preferably from 23 to 31 %. most preferably from 23.3 to 31.0 %; a degree of amidation (DA) of from 5 to 30 %, more preferably from 12 to 25 %, even more preferably from 15 to 23 %, most preferably from 22. 1 to 16.0 %, and, a ratio of a degree of esterification (DE) to a degree of amidation (DA) of from 0.75 to 3.0, preferably from 0.85 to 2.5, more preferably from 0.95 to 2.0, most preferably from 1.05 to 1.94.
  • DE degree of esterification
  • DA degree of amidation
  • the pectin in the composition has a degree of esterification (DE) of from 23.3 to 31 %. a degree of amidation (DA) of from 16.0 to 22. 1 %, and, a ratio of a degree of esterification (DE) to a degree of amidation (DA) of from 1.05 to 1.94.
  • DE degree of esterification
  • DA degree of amidation
  • DA degree of amidation
  • the composition may comprise a pectin and water, wherein the critical gelling concentration (Co) is from 0.05 to 0.12 weight %, and preferably wherein the pectin has a ratio of a degree of esterification (DE) to a degree of amidation (DA) of from 1.05 to 1.94.
  • the critical gelling concentration (Co) is from 0.05 to 0.12 weight %, and preferably wherein the pectin has a ratio of a degree of esterification (DE) to a degree of amidation (DA) of from 1.05 to 1.94.
  • the pectin may be sourced from any one of apples, apple pomace, citrus fruits, citrus peel, lemons, mandarin oranges, grapefruit, sweet orange, pomelo, clementines, limes, kumquat, bitter oranges, blood oranges, satsumas, yuzus, tangelos, or, any combinations thereof.
  • the composition may comprise apple pectin, for example pectin extracted from apple pomace.
  • the composition may comprise apple pectin and water, wherein the critical gelling concentration (Co) is 0. 12 weight %, and preferably wherein the pectin has a ratio of a degree of esterification (DE) to a degree of amidation (DA) of from 1.94.
  • the entire amount of pectin present in the composition is apple pectin.
  • the composition may comprise citrus pectin, for example pectin extracted from citrus fruits, e.g., citrus peel.
  • the composition may comprise citrus pectin and water, wherein the critical gelling concentration (Co) is 0.05 weight %, and preferably wherein the pectin has a ratio of a degree of esterification (DE) to a degree of amidation (DA) of 1.05.
  • the entire amount of pectin present in the composition is citrus pectin.
  • the degree of esterification and the degree of amidation may be measured by titration techniques.
  • the pectin in the composition may be homogeneous.
  • the composition comprises pectin and water, wherein the pectin is preferably extracted from a single pectin source, said pectin source being chosen from the group consisting of apples, apple pomace, citrus fruits, citrus peel, lemons, mandarin oranges, grapefruit, sweet orange, pomelo, clementines, limes, kumquat, bitter oranges, blood oranges, satsumas, yuzus. tangelos, or. any combinations thereof.
  • the composition consists of a pectin and water, preferably, wherein the pectin is homogeneously distributed inside the water.
  • the pectin in the composition may be amidated.
  • the pectin in the composition may be a LM amidated pectin.
  • the composition may comprise sugar.
  • the sugar may be. but is not necessarily limited to, sucrose, dextrose, lactose, maltose, glucose and/or galactose.
  • the sugar is sucrose.
  • the composition comprises the sugar at from 20 to 60 weight %, preferably from 30 to 50 weight %, more preferably from 35 to 45 weight %, most preferably at 40 weight % of the total weight of the composition.
  • composition may additionally comprise a gel-promoting medium and/or a buffer.
  • the gel -promoting medium comprises citric acid monohydrate, tri-sodium citrate dihydrate, sodium benzoate, calcium chloride dihydrate and water.
  • the citric acid monohydrate is present at from 300 to 350 g, more preferably at from 320 to 330 g, most preferably at 325.598 g.
  • the trisodium citrate dihydrate is present at from 150 to 200 g, more preferably from 160 to 170 g, most preferably at 167.493 g.
  • the sodium benzoate is present at from 0.5 to 10 g, more preferably from 3 to 7 g, most preferably at 5 g.
  • the calcium chloride dihydrate is present at from 0.5 to 10 g, more preferably from 4 to 8 g, most preferably at 6.2 g.
  • the distilled water is present at from 4000 to 5000 g, more preferably, at from 4400 to 4600 g, most preferably at 4495.709 g.
  • the citric acid monohydrate is present at 325.598 g
  • the tri-sodium citrate dihydrate is present at 167.493 g
  • the sodium benzoate is present at 5 g
  • the calcium chloride dihydrate is present at 6.2 g
  • the distilled water is present at 4495.709 g.
  • the buffer comprises sodium citrate and water
  • the buffer contains sufficient sodium citrate so that the pH of the buffer is from 3 to 4. more preferably from 3.2 to 3.6, most preferably 3.4.
  • the composition has a critical gelling concentration (Co) wherein the critical gelling concentration (Co) varies by from 0.01 to 0.2 weight %, wherein the composition further comprises a gel-promoting medium and a buffer; wherein the gel-promoting medium comprises citric acid monohydrate, tri-sodium citrate dihydrate, sodium benzoate, calcium chloride dihydrate and water; and wherein the buffer comprises sodium citrate and water.
  • the critical gelling concentration (Co) varies by from 0.01 to 0.2 weight %
  • the composition further comprises a gel-promoting medium and a buffer; wherein the gel-promoting medium comprises citric acid monohydrate, tri-sodium citrate dihydrate, sodium benzoate, calcium chloride dihydrate and water; and wherein the buffer comprises sodium citrate and water.
  • composition Temperature of gelation and critical gelling concentration
  • the composition comprises a pectin and water.
  • the pectin is present in the composition in an amount of from 0.001 to 10 weight % relative to the total amount of pectin and water, preferably from 0.01 to 7.5 weight % relative to the total amount of pectin and water, more preferably from 0. 1 to 5 weight % relative to the total amount of pectin and water, even more preferably from 0.2 to 3 weight % relative to the total amount of pectin and water, even more preferably from 0.3 to 2.5 weight % relative to the total amount of pectin and water, most preferably from 0.4 to 2 weight % relative to the total amount of pectin and water.
  • the composition has a temperature of gelation (Tg) and a critical gelling concentration (Co), wherein when the concentration of the pectin relative to the total amount of pectin and water is increased from 0.8 weight % to 1.4 weight %, the temperature of gelation (Tg) varies by from 0.5 to 2.5°C preferably from 0.5 to 2.0 °C, more preferably from 0.75 to 1.5 °C, even more preferably from 1.0 to 1.3 °C, most preferably from 1.03 to 1.27 °C, and, wherein the critical gelling concentration (Co) is from 0.01 to 0.2 weight %, preferably from 0.02 to 0.17 weight %. more preferably from 0.025 to 0. 15 weight %. even more preferably from 0.04 to 0. 13 weight %, most preferably from 0.05 to 0. 12 weight %.
  • Tg temperature of gelation
  • Co critical gelling concentration
  • the composition may have a temperature of gelation (Tg) and a critical gelling concentration (Co), wherein when the concentration of the pectin relative to the total amount of pectin and water is increased from 0.8 weight % to 1.4 weight %, the temperature of gelation (Tg) varies by from 1.03 to 1.27 °C, and, wherein the critical gelling concentration (Co) is from 0.05 to 0.12 weight %.
  • Tg temperature of gelation
  • Co critical gelling concentration
  • the pectin in the composition has a degree of amidation (DA) of from 5 to 30 %, more preferably from 12 to 25 %, even more preferably from 15 to 23 %, most preferably 16.0 to 22.1 %.
  • DA degree of amidation
  • the pectin in the composition may have a ratio of a degree of esterification (DE) to a degree of amidation (DA) of from 0.75 to 3.0, preferably from 0.85 to 2.5, more preferably from 0.95 to 2.0, even most preferably from 1.05 to 1.94.
  • DE degree of esterification
  • DA degree of amidation
  • the pectin in the composition has a degree of esterification (DE) of from 15 to 45 %, more preferably from 18 to 40 %, even more preferably from 20 to 35 %, even more preferably from 23 to 31 %, most preferably from 23.3 to 31.0 %; a degree of amidation (DA) of from 5 to 30 %, more preferably from 12 to 25 %, even more preferably from 15 to 23 %. most preferably from 16.0 to 22. 1 %, and. a ratio of a degree of esterification (DE) to a degree of amidation (DA) of from 0.75 to 3.0, preferably from 0.85 to 2.5. more preferably from 0.95 to 2.0, most preferably from 1.05 to 1.94.
  • DE degree of esterification
  • DA degree of amidation
  • the pectin in the composition has a degree of esterification (DE) of from 23.3 to 31 %, a degree of amidation (DA) of from 16.0 to 22. 1 %, and. a ratio of a degree of esterification (DE) to a degree of amidation (DA) of from 1.05 to 1.94.
  • DE degree of esterification
  • DA degree of amidation
  • DA degree of amidation
  • the pectin may be sourced from any one of apples, apple pomace, citrus fruits, citrus peel, lemons, mandarin oranges, grapefruit, sweet orange, pomelo, clementines, limes, kumquat, bitter oranges, blood oranges, satsumas, yuzus. tangelos, or. any combinations thereof.
  • the degree of esterification and the degree of amidation may be measured by titration techniques.
  • the pectin in the composition may be homogeneous.
  • the composition comprises pectin and water, wherein the pectin is preferably extracted from a single pectin source, said pectin source being chosen from the group consisting of apples, apple pomace, citrus fruits, citrus peel, lemons, mandarin oranges, grapefruit, sweet orange, pomelo, clementines, limes, kumquat, bitter oranges, blood oranges, satsumas, yuzus, tangelos, or, any combinations thereof.
  • the composition consists of a pectin and water, preferably, wherein the pectin is homogeneously distributed inside the water.
  • the pectin in the composition may be amidated.
  • the pectin in the composition may be a LM amidated pectin.
  • the composition may comprise sugar.
  • the sugar may be, but is not necessarily limited to, sucrose, dextrose, lactose, maltose, glucose and/or galactose.
  • the sugar is sucrose.
  • the composition comprises the sugar at from 20 to 60 weight %, preferably from 30 to 50 weight %, more preferably from 35 to 45 weight %. most preferably at 40 weight % of the total weight of the composition.
  • the composition may additionally comprise a gel-promoting medium and/or a buffer.
  • the gel-promoting medium comprises citric acid monohydrate, tri-sodium citrate dihydrate, sodium benzoate, calcium chloride dihydrate and water.
  • the citric acid monohydrate is present at from 300 to 350 g, more preferably at from 320 to 330 g, most preferably at 325.598 g.
  • the trisodium citrate dihydrate is present at from 150 to 200 g, more preferably from 160 to 170 g, most preferably at 167.493 g.
  • the sodium benzoate is present at from 0.5 to 10 g, more preferably from 3 to 7 g, most preferably at 5 g.
  • the calcium chloride dihydrate is present at from 0.5 to 10 g, more preferably from 4 to 8 g, most preferably at 6.2 g.
  • the distilled water is present at from 4000 to 5000 g, more preferably, at from 4400 to 4600 g, most preferably at 4495.709 g.
  • the citric acid monohydrate is present at 325.598 g
  • the tri-sodium citrate dihydrate is present at 167.493 g
  • the sodium benzoate is present at 5 g
  • the calcium chloride dihydrate is present at 6.2 g
  • the distilled water is present at 4495.709 g.
  • the buffer comprises sodium citrate and water
  • the buffer contains sufficient sodium citrate so that the pH of the buffer is from 3 to 4. more preferably from 3.2 to 3.6, most preferably 3.4.
  • the composition has a temperature of gelation (Tg) and a critical gelling concentration (Co), wherein when the concentration of the pectin relative to the total amount of pectin and water is increased from 0.8 weight % to 1 .4 weight %, the temperature of gelation (Tg) varies by from 0.5 to 2.5°C; wherein the critical gelling concentration (Co) is from 0.01 to 0.2 weight %; wherein the composition further comprises a gel-promoting medium and a buffer; wherein the gel-promoting medium comprises citric acid monohydrate, tri-sodium citrate dihydrate, sodium benzoate, calcium chloride dihydrate and water; and wherein the buffer comprises sodium citrate and water.
  • Tg temperature of gelation
  • Co critical gelling concentration
  • composition as a pectin gel
  • composition as set out under the heading “Composition” can be in the form of a pectin gel.
  • Pectin gels according to the presently described invention have various desirable properties, which make these pectin gels useful in various food and beverage products.
  • the pectin gel comprises the composition as set out under the heading "Composition", i.e.. the pectin gel comprises water and pectin.
  • the pectin is present in the pectin gel in an amount of from 0.001 to 10 weight % relative to the total amount of pectin gel, preferably from 0.01 to 7.5 weight % relative to the total amount of pectin gel, more preferably from 0. 1 to 5 weight % relative to the total amount of pectin gel, even more preferably from 0.2 to 3 weight % relative to the total amount of pectin gel, even more preferably from 0.3 to 2.5 weight % relative to the total amount of pectin gel, most preferably from 0.4 to 2 weight % relative to the total amount of pectin gel.
  • the pectin gel may further comprise an additional material which is, but not limited to, sucrose, glucose, fructose, ribose, glyceraldehyde, lactose, maltose, glycerol, erythritol, sorbitol, xylitol, mannitol, lactitol, maltitol, or any combinations thereof.
  • the pectin gel comprises the additional material at from 20 to 60 weight %, preferably from 30 to 50 weight %, more preferably from 35 to 45 weight %, most preferably at 40 weight % of the total weight of the pectin gel.
  • the pectin gel may further comprise fragrants, flavourants, colourants, preservatives and the like.
  • the pectin gel may comprise gel-promoting mediums, such as but not limited to calcium.
  • the pectin gel may comprise one or more immiscible materials dispersed throughout the pectin gel.
  • the water immiscible material is dispersed in the gel in the form of an emulsion.
  • the water immiscible material is a volatile organic component such as an oil, or, an organic oil immiscible in water, or, an aqueous matrix.
  • the water immiscible material is, but not limited to, perfume, flavourant, pheromone, bactericide, insect attractant, insect repellent, animal attractant, animal repellent, insecticide, fungicide, pharmaceutical drug, veterinary drug, other volatile oils or organic materials, or any combinations thereof.
  • Another aspect of the present invention relates to the method of making a pectin.
  • this aspect of the present invention relates to a method of making a LM amidated pectin.
  • HM pectin is first extracted from citrus peel or apple pomace. The extracted HM pectin then undergoes amidation to form a LM amidated pectin.
  • FIG. 1 depicts a flow diagram for method 1.
  • Step 1 Extraction of HM pectin from a natural source of pectin
  • a natural source of pectin is mixed in acidic, hot water to extract the HM pectin from the natural source of pectin in aqueous form following the methodology described elsewhere such as in Endreb, H.-U., & Christensen, S. H. (2020). Pectins. In G. O. Philips & P. A. Williams (Eds.). Handbook of hydrocolloids (3rd ed.. pp. 274-297). Cambridge: Woodhead Publishing Limited, the disclosure of which is hereby incorporated by reference in its entirety.
  • the natural source of pectin is a raw material extracted from fruit.
  • the natural source of pectin can be fruits such as apples, apple pomace, pears, plums, guavas, quince, gooseberries and citrus fruits such as citrus peel, lemons, mandarin oranges, grapefruit, sweet orange, pomelo, clementines, limes, kumquat, bitter oranges, blood oranges, satsumas, yuzus, tangelos, or, any combinations thereof.
  • the fruit extract is sourced from apple pomace and/or citrus peel.
  • the temperature of the acidic, hot water is from 60 to 80°C, or, from 65 to 75°C, or, from 68 to 72°C.
  • the pH of the acidic, hot water is from pH 1 to 2, or, from pH 1.25 to 1.95, or, from pH 1.4 to 1.8, or, from pH 1.45 to 1.75, or, from pH 1.50 to 1.70.
  • the residence time of the fruit extract in the acidic, hot water is from 1 to 20 hours, or, from 6 to 14 hours, or, from 7 to 13 hours, or, from 8 to 12 hours.
  • the temperature of the acidic, hot water is from 68 to 72°C
  • the pH of the acidic, hot water is from pH 1.50 to 1.70
  • the residence time of the fruit extract in the acidic, hot water is from 8 to 12 hours.
  • HM pectin in aqueous form may then be clarified by using centrifugation, filtration or other conventional separation technologies known in the art to obtain a clarified HM pectin in aqueous form.
  • the clarified HM pectin in aqueous form may then be concentrated to form a concentrated HM pectin in aqueous form by using any technique known in the art.
  • An alcohol may be added to the concentrated HM pectin in aqueous form to cause the HM extract to precipitate out as a precipitate containing the HM pectin.
  • the amount of alcohol added depends on the amount of alcohol required to cause the clarified HM extract to precipitate out from its aqueous form as a precipitate containing the HM pectin.
  • the alcohol used is one or more of isopropanol, tert-amyl alcohol, benzy l alcohol , 1,4-butanediol, 1, 2, 4-butanetriol, butanol, 1 -butanol, 2-butanol, tert-butyl alcohol, diethylene glycol, ethanol, ethylene glycol, 2-ethylhexanol, furfuryl alcohol, glycerol, iso-butanol, isopropyl alcohol, methanol.
  • 2-(2-methoxyethoxyl)ethanol 2-methyl-l -butanol, 2- methyl-1 -pentanol, 3-methyl-2-butanol, neopentyl alcohol, 2-pentanol, 1,3-propanedioL propan- l-ol, propylene glycol, propylene glycol methyl ether, or, any combination thereof.
  • the alcohol is isopropyl alcohol.
  • the precipitate containing the HM pectin may be separated from the alcohol/ water mix.
  • the precipitate containing the HM pectin is separated from the alcohol/ water mix by mechanical separation, wherein any mechanical separation known in the art can be used.
  • the precipitate containing the HM pectin obtained from the separation is washed with alcohol to form a washed precipitate containing the HM pectin.
  • the alcohol used is one or more of isopropanol, tert-amyl alcohol, benzyl alcohol , 1,4-butanediol, 1, 2, 4-butanetriol, butanol, 1 -butanol, 2-butanol, tert-butyl alcohol, diethylene glycol, ethanol, ethylene glycol, 2-ethylhexanol, furfuryl alcohol, glycerol, iso-butanol, isopropyl alcohol, methanol.
  • 2-(2-methoxyethoxyl)ethanol 2 -methyl- 1 -butanol, 2- methyl-1 -pentanol, 3-methyl-2-butanol, neopentyl alcohol, 2-pentanol, 1,3 -propanediol, propan- l-ol, propylene glycol, propylene glycol methyl ether, or, any combination thereof.
  • the alcohol is isopropyl alcohol.
  • the precipitate containing the HM amidated pectin obtained from the separation is washed with the alcohol one, two, three, four, five, six, seven, eight, nine, ten, or more than ten times.
  • the HM amidated pectin is washed with the alcohol three times.
  • the precipitate containing the HM amidated pectin obtained from the separation is washed with alcohol at from 50 to 70 weight %, or, from 55 to 65 weight %, or, at 60 weight % of the total weight of the alcohol to form a washed HM pectin.
  • the alcohol used is one or more of isopropanol, tert-amyl alcohol, benzyl alcohol . 1,4-butanediol. 1, 2, 4-butanetrioL butanol, 1 -butanol.
  • the alcohol is isopropyl alcohol.
  • the washed HM pectin may then undergo a drying step to form a dry HM pectin.
  • the drying step dries the washed HM pectin until the washed HM pectin has a moisture content of from 5 to 15 weight %, or, from 7.5 to 12.5 weight %, or, 10 weight % of the total weight of the dry HM pectin.
  • the drying step is carried out by press-drying.
  • the product of the dry ing step is a dry HM pectin.
  • the dry HM pectin can be ground until a homogeneous particle size distribution is achieved.
  • the dry HM pectin can be blended with sugar to form a standardised HM pectin.
  • Step 2 Amidation of dry HM pectin
  • the dry HM pectin may be placed in a suspension which comprises alcohol and ammonia to form an amidated LM pectin.
  • the alcohol used is one or more of isopropanol, tert-amyl alcohol, benzyl alcohol . 1,4-butanediol. 1, 2, 4-butanetriol. butanol, 1 -butanol.
  • the alcohol is isopropyl alcohol.
  • the alcohol is present at from 50 to 80 weight %, or, from 55 to 75 weight %, or, from 60 to 70 weight % of the total weight of the suspension.
  • the alcohol is present at from 60 to 70 weight % of the total weight of the suspension.
  • the ammonia is present at from 2 to 4 weight %, or, from 2.5 to 3.75 weight %, or, from 2.8 to 3.5 weight % of the total weight of the suspension.
  • the ammonia is present at from 2.8 to 3.5 weight % of the total weight of the suspension.
  • the suspension is maintained at a temperature of from 5 to 20 °C, or, from 8 to 16 °C , or, from 9 to 15 °C, or, from 10 to 14 °C.
  • the suspension is maintained at a temperature of from 10 to 14 °C.
  • the dry 7 HM pectin is maintained in the suspension for from 3 to 10 hours, or, from 4 to 9 hours, or, from 5 to 8 hours.
  • the dry HM pectin is maintained in the suspension for from 5 to 8 hours.
  • the alcohol is present at from 60 to 70 weight % of the total weight of the suspension
  • the ammonia is present at from 2.8 to 3.5 weight % of the total weight of the suspension
  • the suspension is maintained at a temperature of from 10 to 14 °C
  • the dry HM pectin is maintained in the suspension for from 5 to 8 hours and the alcohol used is isopropyl alcohol.
  • the LM amidated pectin can be filtered out of the suspension to produce a filtrate comprising the alcohol and a residue comprising the LM amidated pectin.
  • the LM amidated pectin can be filtered out of the suspension by any filtration technique known in the art.
  • the filtrate comprising the alcohol and ammonia pass to a recovery step.
  • the residue comprising the LM amidated pectin can be washed to form a w ashed LM amidated pectin.
  • the residue comprising the LM amidated pectin is washed with alcohol.
  • the residue comprising the LM amidated pectin is washed with alcohol at from 50 to 70 weight %, or, from 55 to 65 weight %, or, at 60 weight % of the total weight of the alcohol.
  • the alcohol used is isopropyl alcohol.
  • the alcohol used is one or more of isopropanol, tert-amyl alcohol, benzyl alcohol , 1,4-butanediol, 1, 2, 4-butanetriol.
  • butanol 1 -butanol.
  • 2-butanol, tert-butyl alcohol di ethylene glycol, ethanol, ethylene glycol.
  • the alcohol is isopropyl alcohol.
  • the pH of the washed LM amidated pectin can be adjusted until the pH lies from 3.0 to 5.5, or, from 3.5 to 4.0, or, from 4.0 to 4.5.
  • the pH of the washed LM amidated pectin is adjusted with acid to form a pH adjusted LM amidated pectin.
  • the acid is nitric acid.
  • the pH adjusted LM amidated pectin may be washed with alcohol to form a second-washed LM amidated pectin.
  • the alcohol is any one of tert-amyl alcohol, benzy l alcohol , 1,4- butanediol, 1, 2, 4-butanetriol, butanol, 1 -butanol, 2-butanol, tert-butyl alcohol, diethylene glycol, ethanol, ethylene glycol, 2-ethylhexanol, furfuryl alcohol, glycerol, iso-butanol, isopropyl alcohol, methanol, 2-(2-methoxyethoxyl)ethanol, 2-methyl-l -butanol, 2-methyl-l- pentanol, 3-methyl-2-butanol, neopentyl alcohol, 2-pentanol, 1,3-propanediol, propan-l-ol, propylene glycol, propylene glycol methyl ether, isopropanol, or, any combination thereof.
  • the alcohol is isopropyl alcohol.
  • the neutralised LM ami dated pectin is washed with the alcohol one, two, three, four, five, six, seven, eight, nine, ten, or more than ten times.
  • the neutralised LM amidated pectin is washed with the alcohol three times.
  • the pH adjusted LM amidated pectin is washed with alcohol at from 50 to 70 weight %, or, from 55 to 65 weight %, or, at 60 weight % of the total weight of the alcohol.
  • the second-washed LM amidated pectin can undergo a drying step to form a dried LM amidated pectin.
  • the drying step is carried out by press-drying.
  • the second-washed LM amidated pectin can be dried until the dried LM amidated pectin has a moisture content of from 1 to 30 weight %, or from 2 to 20 weight &, or from 7.5 to 15.0 weight 5, or from 9 to 11 weight %, or. 10 weight % of the total weight of the dried LM amidated pectin.
  • the dried LM amidated pectin is a LM amidated pectin ready for use in a composition according to the present invention.
  • the dried LM amidated pectin can be blended with sugar to form a standardised LM amidated pectin.
  • the product of the second step to be the pectin of the present invention
  • some key parameters of the above process need to be controlled in the amidation reaction.
  • the parameters include the of alcohol and ammonia weight % in the suspension, the residence time of the HM pectin in the suspension and the temperature of the suspension. By controlling these parameters, the desired degree of esterification and degree of amidation can be obtained.
  • the weight % of the ammonia in the suspension is at from 2.8 to 3.5 weight % of the total weight of the suspension.
  • the w eight % of the weight % of the alcohol in the suspension is 60 to 70 weight % of the total weight of the suspension
  • the residence time is maintained for from 5 to 8 hours.
  • the reaction temperature is maintained at from 10 to 14°C.
  • weight % of the ammonia in the suspension is at from 2.8 to 3.5 weight % of the total weight of the suspension
  • the weight % of the alcohol in the suspension is 60 to 70 weight % of the total weight of the suspension
  • the residence time is maintained for from 5 to 8 hours and the reaction temperature is maintained at from 10 to 14°C.
  • composition comprising a pectin
  • composition comprises a pectin and water.
  • the method of making the composition comprises the following steps:
  • the composition may comprise the pectin at a concentration of from 0.001 to 10 weight % relative to the total amount of pectin and water, preferably from 0.01 to 7.5 weight % relative to the total amount of pectin and water, more preferably from 0.1 to 5 weight % relative to the total amount of pectin and water, even more preferably from 0.2 to 3 weight % relative to the total amount of pectin and water, even more preferably from 0.3 to 2.5 weight % relative to the total amount of pectin and water, most preferably from 0.4 to 2 weight % relative to the total amount of pectin and water.
  • the composition may additionally comprise a gel-promoting medium at from 0.001 to 10 mM, preferably from 0.005 to mM, most preferably from 0.01 to 8 mM.
  • a gel-promoting medium is calcium.
  • the composition comprises pectin at a concentration of from 0.4 to 2 weight % of the total weight of the composition and calcium (as a gel-promoting medium) at from 0.01 to 8 mM.
  • the composition may additionally comprise sugar.
  • the composition may comprise the sugar at from 20 to 60 weight %, or, from 30 to 50 weight %, or, from 35 to 45 weight %, or at 40 weight % of the total weight of the composition.
  • the sugar is, but not limited to. sucrose, dextrose, lactose, maltose, glucose and/or galactose.
  • the pectin is at a concentration of from 0.001 to 10 weight % of the total weight of the pectin gel. preferably from 0.01 to 7.5 weight % of the total weight of the pectin gel, more preferably from 0.1 to 5 weight % of the total weight of the pectin gel, even more preferably from 0.2 to 3 weight % of the total weight of the pectin gel, even more preferably from 0.3 to 2.5 weight % of the total weight of the pectin gel, most preferably from 0.4 to 2 weight % of the total weight of the pectin gel.
  • the gel-promoting medium is at a concentration of from 0.001 to 10 mM, preferably from 0.005 to 9 mM, most preferably from 0.01 to 8 mM.
  • the gel-promoting medium is calcium.
  • the pectin is at a concentration of from 0.4 to 2 weight % of the total weight of the pectin gel and the gelmedium cation is at a concentration of from 0.01 to 8 mM.
  • the solution is heated to from 70 to 110 °C, preferably from 75 to 105 °C, most preferably from 80 to 95 °C.
  • the solution is heated from a duration of from 1 to 60 minutes, preferably from 5 to 45 minutes, most preferably from 10 to 30 minutes.
  • the solution is heated to from 80 to 95 °C for a duration of 10 to 30 minutes.
  • the solution is cooled to a temperature of from 1 to 30 °C, preferably from 5 to 25 °C. most preferably from 10 to 20 °C.
  • the composition may be incorporated into a daily' product, which includes, but is not limited to, milk, condensed milk, dried milk, milk-drinks, cream, butter, yoghurt, cheese, custard, cottage cheese, cream cheese, curd, frozen dairy products such as frozen custard, frozen yogurt and ice-cream, gelato, powdered milk, evaporated milk, sour cream, soured milk, whey, whey protein or whipped cream.
  • a daily' product includes, but is not limited to, milk, condensed milk, dried milk, milk-drinks, cream, butter, yoghurt, cheese, custard, cottage cheese, cream cheese, curd, frozen dairy products such as frozen custard, frozen yogurt and ice-cream, gelato, powdered milk, evaporated milk, sour cream, soured milk, whey, whey protein or whipped cream.
  • composition may be incorporated into a sweet product, which includes, but is not limited to, a confectionary product, reduced sugar jams, fruit preparations, jellies, glazes and spray glazes.
  • the composition is incorporated into a meat product, a poultry’ product, a fish product, dairy products such as milk, ice cream, yoghurt, cheese, pudding, and flavoured dairy drinks, baked foods such as bread, cake, cookies, crackers, biscuits, pies, donuts, pretzels, and potato chips, non-dairy spreads, mayonnaise, soups, sauces, dips, dressings, frozen confections, fruit preparations, jams and jellies, beverages, water gels, confectionery jelly or low-fat spreads.
  • dairy products such as milk, ice cream, yoghurt, cheese, pudding, and flavoured dairy drinks
  • baked foods such as bread, cake, cookies, crackers, biscuits, pies, donuts, pretzels, and potato chips
  • non-dairy spreads mayonnaise, soups, sauces, dips, dressings, frozen confections, fruit preparations, jams and jellies, beverages, water gels, confectionery jelly or low-fat spreads.
  • composition in a non-food or non-beverage product is a non-food or non-beverage product
  • composition in a non-food or a non-beverage product, wherein the composition is as set out under the heading “Composition”.
  • composition may be incorporated into other products related to nutraceuticals, biological activities, cosmetics and pharmaceutics.
  • composition a food or beverage product comprising the composition, wherein the composition is as set out under the heading “Composition’”.
  • the method of making the food or beverage product comprises the steps:
  • Another aspect of the present invention relates to a method of making a non-food or non-beverage product comprising the composition, wherein the composition is as set out under the heading “Composition”.
  • the method of making the non-food or non-beverage product comprises the steps:
  • novel pectins were compared to commercially available pectins, provided by Cargill, Incorporated.
  • Pectin samples are listed in Table 1.
  • Table 1 Pectin samples used in the evaluation of the present invention.
  • Table 2 The composition of the commercially available pectins.
  • GalA is the galacturonic acid (GalA) content of each pectin.
  • citrus peel or apple pomace was mixed in acidic, hot water to extract the HM pectin from the citrus peel or apple pomace as a HM pectin in aqueous form.
  • the temperature of the acidic, hot water was from 68 to 72°C, the pH was from pH 1.50 to 1.70 and the residence time was from 8 to 12 hours.
  • HM pectin in aqueous form was clarified by using centrifugation and filtered to form a clarified HM pectin in aqueous form.
  • the washed HM pectin then underw ent a drying step to form a dry HM pectin.
  • the drying step dried the washed precipitate containing the HM pectin until the washed precipitate containing the HM pectin had a moisture content of 10 weight % of the total weight of the dry HM pectin.
  • the dry HM pectin was placed in a suspension which comprised alcohol (isopropyl alcohol) and ammonia.
  • the alcohol was present at from 60 to 70 weight % of the total weight of the suspension and the ammonia was present at 2.8 to 3.5 weight % of the total weight of the suspension.
  • the suspension was maintained at a temperature of from 10 to 14 °C.
  • the dry HM pectin was in the suspension for from 5 to 8 hours. Once 5 to 8 hours had passed, the dry HM pectin had undergone amidation to form LM amidated pectin.
  • the LM amidated pectin was fdtered out from the alcohol and ammonia.
  • the alcohol and ammonia passed to a recover ⁇ ' step.
  • the LM amidated pectin was washed with isopropyl alcohol at 60 weight % of the total weight of the alcohol to form a washed LM amidated pectin.
  • the pH of the washed LM amidated pectin was adjusted to form a pH adjusted LM amidated pectin.
  • the pH of the washed LM amidated pectin w as adj usted until the pH was between 4.0 to 4.5.
  • the pH was adjusted with nitric acid.
  • the second-washed LM amidated pectin underwent a drying step to form a dried LM amidated pectin.
  • the drying step dried the second-washed LM amidated pectin until the second-washed LM amidated pectin had a moisture content of 10 weight % of the total w eight of the dried LM amidated pectin.
  • Example 2 Structural characterisation of a LM amidated pectin
  • the degree of esterification (DE), degree of amidation (DA) and galacturonic acid content (GalA) of a pectin were determined using a titration method (as set out in National Research Council, 1981, Yu, et al, 2021, the disclosure of which is hereby incorporated by reference in its entirety).
  • the method of measuring the degree of esterification (DE), degree of amidation (DA) and galacturonic acid content (GalA) includes washing the pectin samples with acidified aqueous isopropanol to remove any cations, salts and standardising sugars. The purified pectin is then titrated with 0.1 M sodium hydroxide.
  • the ester groups are saponified with an excess of 0.5 M sodium hydroxide, which is then neutralised with an exactly equivalent amount of 0.5 M hydrochloric acid, enabling the liberated acid groups to be titrated with 0.1 M sodium hydroxide.
  • the solution may then be distilled with strong alkali to liberate ammonia from the amide groups of amidated pectins.
  • the ammonia is estimated in terms of the same 0.1 M sodium hydroxide.
  • the proportions of the degree of amidation, the degree of esterification and galacturonic acid content were calculated following the procedure described in National Research Council, 1981, Yu, et al, 2021, the disclosure of which is hereby incorporated by reference in its entirety.
  • Table 3 The chemical composition of the pectin.
  • Example 3 Measuring the intrinsic viscosity of the LM amidated pectin
  • the intrinsic viscosity of the pectins was determined by size-exclusion chromatography-Multi-Angle Laser Light Scattering (SEC-MALLS) as descnbed in Hellin, P complicat Ralet, M. C , Bonnin, E Cincinnati & Thibault, J. F. (2005).
  • Homogalacturonans from lime pectins exhibit homogeneous charge density and molar mass distributions.
  • Pectin solutions at 5 mg/mL in water were prepared in 50 mM sodium nitrate containing 0.02 weight % sodium azide as a preservative.
  • the intrinsic viscosity was calculated using Astra software (Wyatt, Santa Barbara, CA, the disclosure of which is hereby incorporated by reference in its entirety) and the TriSec software (Version 3.0, Voscotek. Houston. TX, the disclosure of which is hereby incorporated by reference in its entirety). All analysis was performed in triplicate, and the mean value taken.
  • Example 4 Makins a composition comprising a LM amidated pectin and water
  • compositions comprising each pectin as shown in Table 1 were made.
  • the compositions comprised pectin and water: each composition comprised one of pectins 1-5.
  • the compositions were prepared so that the resultant pectin concentrations were at from 0.4 to 2.0 weight % with sucrose (at 40 weight %) of the total weight of the composition.
  • each composition pre-solutions of pectin were first prepared by dissolving each pectin separately in distilled water under mechanical stirring for 10 minutes at 90°C. [000193] After dissolution of the pectin in the distilled water, from 190 to 320 g of a hot buffer solution and a gel-promoting medium were added to the distilled water and pectin solution.
  • the buffer comprised sodium citrate at a sufficient concentration so that the pH of the buffer was at 3.4.
  • the sodium citrate was dissolved in distilled water. Prior to adding the buffer to the distilled water and pectin solution, the buffer was heated to the same temperature as the distilled water and pectin solution (90°C).
  • the buffer solution also contained CaCh (at 8.4 mM) and sucrose.
  • the gel-promoting medium was added to the solution comprising the distilled water and pectin at a concentration of 8.4 mM in water.
  • the composition of the gel-promoting medium is set out in Table 5.
  • the ionic strength of the gel -promoting medium plays an important role on the temperature of gelation critical gelling concentration.
  • the resulting composition having a final calcium chloride (CaCh) concentration of 3 mM, was kept under stirring (at 90°C) for 5 minutes.
  • the final pH of each composition prepared was 3.4.
  • Table 6 The pectin used to make each composition.
  • the temperature of gelation (Tg) was measured for each composition.
  • the temperature of gelation (Tg) was measured over a pectin concentration ranging from 0.8 weight % to 1.4 weight % (of the total weight of the composition) for each composition.
  • compositions analysed are the compositions produced in Example 4.
  • Tg temperature of gelation
  • MCR 92 stress-controlled rheometer Anton Paar Physica
  • each composition (as described above in Example 4) was covered by a thin layer of paraffin oil to avoid evaporation during measurements.
  • each composition was poured (separately) into the Couette device (pre-heated at 80°C) and was first pre-sheared (at 10 s’ 1 for 2 min) to clean the loading history of the composition. The composition was then exposed to a temperature sweep test (2°C/min) from 80°C down to 10°C.
  • the viscoelastic experiments performed using the ARES-G2 strain-controlled rheometer and the MCR 92 stress-controlled rheometer were carried out at 0.4% and 10% of strain, respectively, and at a frequency of 0.8 Hz. Both strain amplitudes were verified to be in the LVE domain.
  • each measurement was performed in triplicate, from new composition preparations (of the same composition). The mean value was taken from the triplicate measurements.
  • the gelation temperature (Tg) representing the cross-over point between storage modulus (G’) and loss modulus (G ”) was collected from the gelation kinetic data obtained after the temperature sweep test (described above).
  • the storage modulus G’ and loss modulus (G : ’) values were collected from the mechanical spectra using an automatic data exporting program from the Rheocompass software (from Anton Paar company).
  • the cross-over point between the storage modulus (G’) and loss modulus (G’’ was determined, as illustrated in FIG. 2.
  • FIG. 2 shows data points for Composition 1 at 1.4 % pectin concentration in water. Then, the mean value of Tg and corresponding standard deviation of the obtained data in triplicate was calculated.
  • Table 7 The mean value for the temperature of gelation (Tg) for each composition.
  • the critical gelling concentration was measured for each composition.
  • the compositions analysed are the compositions produced in Example 4.
  • each composition prepared as described above was covered by a thin layer of paraffin oil to avoid evaporation during measurements.
  • each composition was poured (separately) into the Couette device (pre-heated at 80°C) and was first pre-sheared (at 10 s' 1 for 2 min) to clean the loading history of the device.
  • Each composition was then exposed to a temperature sweep test (2°C/min) from 80°C down to 10°C. followed by a time sweep experiment for 30 minutes at a frequency of 0.8 Hz to ensure that the resulting gel reaches an equilibrium state due to reorganization (structural rearrangements).
  • strain sweep experiments were conducted from 0.01% to 40% at 0.8 Hz.
  • R 2 is a statistical measure of fit that indicates how much variation of a dependent variable is explained by the independent values in a regression model: when R 2 is close to one (as with this case), the fitting model is robust);
  • Table 8 The mean value of the critical gelling concentration (Co) for each composition.
  • a low critical gelling concentration (Co) results in a highly functional product.
  • the lower the critical gelling concentration (Co) of the composition the less of the composition that is required in a food and/or beverage product to obtain a gel.
  • the compositions of the present invention have a low critical gelling concentration (Co) and therefore less of the composition will be required in a food and/or beverage product to obtain a gel. This advantageously results in a food and/or beverage product which is cheaper to manufacture, because less of the composition is required in the food and/or beverage product.
  • the above-mentioned advantage for end-used product formulation can help identify novel routes of rational product formulation (thus allowing the cost-in-use to be reduced) and continuously optimises pectin processing conditions.

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Abstract

The present invention relates to a composition comprising a pectin and water, and a method of making the composition. In particular, the present invention relates to a composition comprising a pectin and water, wherein when the concentration of the pectin in the water is increased from 0.8 weight % to 1.4 weight % relative to the total weight of the composition, the temperature of gelation (Tg) varies by from 0.5 to 2.5 °C. The composition has properties useful to the food and/or beverage industry.

Description

A COMPOSITION COMPRISING A PECTIN AND WATER
CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application claims the benefit of European Patent Application No. 23167025.8, filed April 6, 2023, which is incorporated by reference herein in its entirety.
FIELD OF THE INVENTION
[0002] The present invention relates to a composition comprising a pectin and water, and a method of making the composition. The composition has properties useful to the food and/or beverage industry.
BACKGROUND OF THE INVENTION
[0003] Pectin is found naturally in plant cell walls. Although pectin can be extracted from a large number of plants or fruits, the main industrial or conventional sources include citrus peel and apple pomace. The main use of pectin is as a gelling agent, thickening agent, viscosifying agent and/or as a stabiliser in food. As a result, pectin is commonly used in jams, jellies, acid milk beverages and dessert bases as a food additive. Pectin can also be used as dietary fibers and as an effective food emulsifier. Pectin also has potential uses in other fields such as medicine as a carrier for controlled drugs or bioactive release and in many other nonfood applications.
[0004] Pectin is a polysaccharide comprising a chain of galacturonic acid units which are linked by a- 1,4 glycosidic bonds. The galacturonic acid chain may partly be esterified as methyl esters. Though the galacturonic acid chain is the backbone of pectin, other chemicals such as acetyl and methyl ester groups can be incorporated into the chain. These groups can be important for distinguishing between different pectin types. A review of pectin properties and characteristics can be found in D. Gawkowska et al. ‘'Structure-Related Gelling of Pectins and Linking with Other Natural Compounds: A Review” Polymers (Basel), 2018 Jul; 10(7): 762, the disclosure of which is hereby incorporated by reference in its entirety'. [0005] Pectin can be split into two categories by its degree of methylation, which is the percentage of carboxyl groups which have undergone esterification with methanol. The degree of methylation is of great importance for the use of pectins as gelling agents and depending on the degree of methylation, the pectin is classified as either a high methoxyl pectin (HM pectin) or a low methoxyl pectin (LM pectin). If more than 50 percent of the carboxyl groups are methylated then the pectin is a HM pectin, and if less than that degree of methylation has occurred then the pectin is a LM pectin.
[0006] HM pectin is the most commonly used pectin and can be split into two categories: rapid set HM pectin and slow set HM pectin. Rapid set pectin will set faster and at a higher temperature than slow set pectin, and thus is preferable in the production of food and/or beverage products which typically require a certain mouthfeel or the suspension of various particulate matter such as whole or portioned fruits, nuts and the like. Slow set pectin is preferable for food and/or beverage products which do not require the presence of suspended particulate matter. HM pectins can form gels with sugar and acid, forming what is known in the art as low water activity gels or sugar acid pectin gels. Slow set pectin can take from 1 to 2 days to set into a gel. These gels have a 3-dimensional network of pectin molecules in which a solvent (usually water), optionally with the co-solutes of sugar and acid are immobilised resulting in a system that can resist deformation.
[0007] LM pectins differ from HM pectins in that the LM pectins only require the presence of a divalent cation to initiate the reaction that causes the pectin to set into a gel. The most commonly used divalent cation is calcium. In general, the gel forming ability of LM pectins increases with a decreasing degree of methylation.
[0008] Recently, LM pectins have been amidated to form LM amidated pectin. LM ami dated pectin is a modified form of LM pectin in which some of the galacturonic acid units are converted by ammonia into carboxylic amides. In traditional methods of producing LM amidated pectin, a HM pectin needs to be first extracted from its natural source. The HM pectin is converted into LM pectin, which undergoes amidation to form the LM amidated pectin. The conversion of the HM pectin into LM amidated pectin follows the reaction scheme:
RCOOCH3 + NH4OH => RCONH2 + CH3OH +H2O [0009] Known methods of forming LM amidated pectin are set out in US2480710A, EP1517925 and WO98/58968A1, the disclosures of which are hereby incorporated by reference in their entirety.
[00010] A LM amidated pectin is advantageous compared to non-amidated LM pectins because the LM amidated pectin can enlarge the calcium sensitivity tolerance of LM pectins and therefore permit gelation over a wider range of calcium concentrations unlike non-amidated LM pectins. Further advantageously, amidated pectins are typically thermo-reversible: LM amidated pectins can be heated to form a liquid and after cooling solidify again, whereas conventional pectin-gels will remain in liquid form after heating and cooling. Further advantageously, LM amidated pectins can promote the stabilisation of junction zones of pectin gel network structures through additional hydrogen bond formation with the amide groups. Further advantageously, LM amidated pectins display good gelling properties under low-sugar conditions.
[00011] Owing to the number of advantages provided by LM amidated pectins. LM amidated pectins are regularly used in the food and/or drink industry. There is thus a continuous need for improved pectins and compositions comprising the pectins, which can be used in the food and/or beverage industry. In particular, there is a continuous need for improved LM amidated pectins and compositions comprising the LM amidated pectins, which can be used in the food and/or beverage industry.
SUMMARY OF THE INVENTION
[00012] The present invention relates to a composition comprising a pectin and water, and a method of making the composition. The composition has properties useful to the food and/or beverage industry.
[00013] Representative features of the present invention are set out in the following clauses, which stand alone or may be combined, in any combination, with one or more features disclosed in the text and/or figures of the specification.
[00014] The present invention is as set out in the following clauses:
1. A composition having a temperature of gelation (Tg), comprising: a pectin; and, water; wherein when the concentration of the pectin in the water is increased from 0.8 weight % to 1.4 weight % relative to the total weight of the composition, the temperature of gelation (Tg) varies by from 0.5 to 2.5 °C.
2. The composition of clause 1 wherein when the pectin concentration in the water is increased from 0.8 weight % to 1.4 weight % relative to the total weight of the composition, the temperature of gelation (Tg) varies by from 0.50 to 2.0 °C, or, from 0.75 to 1.5 °C, or, from 1.0 to 1.3 °C, or, from 1.03 to 1.27 °C.
3. The composition of clause 1 or clause 2, wherein the pectin has a degree of esterification (DE) of from 15 to 45 %, or from, 18 to 40 %, or, from 20 to 35 %, or, from 23 to 31 %, or, from 23.3 to 31.0 %.
4. The composition of any one of clauses 1 to 3, wherein the pectin has a degree of amidation (DA) of from 5 to 30 %, or, from 12 to 25 %, or, from 15 to 23 %, or, from 16.0 to 22.1 %.
5. The composition of any one of clauses 1 to 4, wherein the pectin has a ratio of a degree of esterification (DE) to a degree of amidation (DA) of from 0.75 to 3.0, or, from 0.85 to 2.5, or. from 0.95 to 2.0, or, from 1 .05 to 1 .94.
6. The composition of any one of clauses 1 to 5, wherein when the pectin concentration in the water is increased from 0.8 weight % to 1.4 weight % relative to the total weight of the composition, the temperature of gelation varies by 1.27°C.
7. The composition of clause 6, wherein the pectin has a ratio of a degree of esterification (DE) to a degree of amidation (DA) of 1.94.
8. The composition of any one of clauses 1 to 5, wherein when the pectin concentration in the water is increased from 0.8 weight % to 1.4 weight % relative to the total weight of the composition, the temperature of gelation varies by 1.03°C. 9. The composition of clause 8, wherein the pectin has a ratio of a degree of esterification (DE) to a degree of amidation (DA) of 1.05.
10. The composition of any one of clauses 1 to 9, wherein the pectin is low methoxyl (LM) amidated pectin; optionally, wherein the low methoxyl (LM) amidated pectin has a degree of methylation of below 50 %.
11. The composition of any one of clauses 1 to 10, wherein the degree of esterification (DE) is measured by titration; and/or, wherein the degree of amidation (DA) is measured by titration; and/or, wherein the temperature of gelation (Tg) is measured by dynamic oscillatory rheological measurements.
12. A pectin having: a degree of esterification (DE) of from 15 to 45 %, or from, 18 to 40 %, or, from 20 to 35 %. or, from 23 to 31 %, or 23.3 to 31 %. a degree of amidation (DA) of from 5 to 30 %, or, from 12 to 25 %, or, from 15 to 23 %, or, from 16 to 22. 1 ; and, a ratio of a degree of esterification (DE) to a degree of amidation (DA) of from 0.75 to 3.0, or, from 0.85 to 2.5, or. from 0.95 to 2.0. or, from 1.05 to 1.94.
13. A composition having a critical gelling concentration (Co) comprising: a pectin; and, water; and wherein the critical gelling concentration (Co) is from 0.01 to 0.2 weight %.
14. The composition of clause 13, wherein the critical gelling concentration (Co) is from 0.02 to 0.17 weight %, or, from 0.025 to 0.15 weight %, or, from 0.04 to 0.13 weight %, or, from 0.05 to 0. 12 weight %.
15. The composition of clause 13 or clause 14, wherein the pectin has a ratio of a degree of esterification (DE) to a degree of amidation (DA) of from 0.75 to 3.0, or, from 0.85 to 2.5, or, from 0.95 to 2.0, or. from 1.05 to 1.94.
16. The composition of any one of clauses 13 to 15, wherein: the critical gelling concentration (Co) is 0.12 weight %: optionally, wherein the pectin has a ratio of a degree of esterification (DE) to a degree of amidation (DA) of 1.94.
17. The composition of any one of clauses 13 to 15, wherein: the critical gelling concentration (Co) is 0.05 weight %; optionally. wherein the pectin has a ratio of a degree of esterification (DE) to a degree of amidation (DA) of 1.05.
18. The composition of any one of clauses 13 to 17, wherein the pectin is a low methoxyl (LM) amidated pectin; optionally, wherein the low methoxyl (LM) amidated pectin has a degree of methylation of below 50 %.
19. The composition of any one of clauses 13 to 18, wherein the degree of esterification (DE) is measured by titration; and/or, wherein the degree of amidation (DA) is measured by titration; and/or, wherein the critical gelling concentration (Co) is measured by dynamic oscillatory rheological measurements.
20. A composition having a temperature of gelation (Tg) and a critical gelling concentration (Co) comprising: a pectin; and, water; wherein when the pectin concentration in the water increases from 0.8 weight % to 1.4 weight % relative to the total weight of the composition, the temperature of gelation (Tg) varies by from 0.5 to 2.5 °C; and wherein the critical gelling concentration (Co) is from 0.01 to 0.2 weight %.
21. The composition of clause 20 wherein when the pectin concentration in the water is increased from 0.8 weight % to 1.4 weight % relative to the total weight of the composition, the temperature of gelation (Tg) varies by from 0.50 to 2.0 °C, or, from 0.75 to 1.5 °C, or, from 1.0 to 1.3 °C, or, from 1.03 to 1.27 °C. 22. The composition of clause 20 or clause 21, wherein the critical gelling concentration (Co) is from 0.02 to 0. 17 weight %, or. from 0.025 to 0. 15 weight %, or, from 0.04 to 0. 13 weight %. or, from 0.05 to 0. 12 weight %.
23. The composition of any one of clauses 20 to 22, wherein the pectin has a ratio of a degree of esterification (DE) to a degree of amidation (DA) of from 0.75 to 3.0, or, from 0.85 to 2.5, or. from 0.95 to 2.0, or. from 1.05 to 1.94.
24. The composition of any one of clauses 20 to 23, wherein the pectin is low methoxyl (LM) ami dated pectin; optionally, wherein the low methoxyl (LM) ami dated pectin has a degree of methylation of below 50 %.
25. The composition of any one of clauses 20 to 24, wherein the degree of esterification (DE) is measured by titration; and/or, wherein the degree of amidation (DA) is measured by titration; and/or, wherein the temperature of gelation (Tg) and/or the critical gelling concentration (Co) is measured by dynamic oscillatory rheological measurements.
26. The composition of any one of clauses 1 to 25, wherein the pectin is sourced from apple pomace and/or citrus peel.
27. The composition of any one of clauses 1 to 26, wherein the composition further comprises sugar, optionally, wherein the sugar is any one of sucrose, dextrose, lactose, maltose, glucose and/or galactose; optionally, wherein the sugar is present at from 20 to 60 weight %, or, from 30 to 50 weight %, or, from 35 to 45 weight %, or at 40 weight % relative to the total weight of the composition.
28. A method of making a composition according to any one of clauses 1 to 27, the method comprising the following steps: obtaining a high methoxyl (HM) pectin in aqueous form from a natural source; dr ing the high methoxyl (HM) pectin in aqueous form to form a dry high methoxyl (HM) pectin, wherein the dry high methoxyl (HM) pectin has a moisture content of 10 weight % of the total weight of the dry high methoxyl (HM) pectin; placing the dry high methoxyl (HM) pectin in a suspension comprising alcohol and ammonia to form an amidated low methoxyl (LM) pectin; drying the amidated low methoxyl (LM) pectin to form a dried amidated low methoxyl (LM) pectin, wherein the dried amidated pectin has a moisture content of 10 weight % of the total weight of the dried amidated low methoxyl (LM) pectin; adding water to the amidated low methoxyl (LM) pectin to form a composition.
29. The method of clause 28, wherein the natural source is any one of apples, apple pomace, citrus peel, lemons, mandarin oranges, grapefruit, sweet orange, pomelo, clementines, limes, kumquat, bitter oranges, blood oranges, satsumas, yuzus. tangelos, or, any combinations thereof.
30. The method of clause 28 or clause 29, wherein the natural source is apple pomace or citrus peel.
31. The method of any one of clauses 28 to 30, further comprising any one or more of the following steps: clarifying the high methoxyl (HM) pectin in aqueous form; optionally wherein the high methoxyl (HM) pectin in aqueous form is clarified by centrifugation and/or filtration; concentrating the high methoxyl (HM) pectin in aqueous form; washing the high methoxyl (HM) pectin in aqueous form with alcohol; subjecting the high methoxyl (HM) pectin in aqueous form to a separation process; optionally, wherein the separation process is mechanical separation. filtering the amidated low methoxyl (LM) pectin; washing the amidated low methoxyl (LM) pectin with alcohol; and/or adjusting the pH of the amidated low methoxyl (LM) pectin.
32. Use of the composition according to any one of clauses 1 to 27 in a food and/or beverage product.
33. A pectin having: a degree of esterification (DE) of from 15 to 45 %; a degree of amidation (DA) of from 5 to 30 %; and a ratio of the degree of esterification (DE) to the degree of amidation (DA) of from 0.5 to
9.0. 34. The pectin of clause 33 having a galacturonic acid content (GalA) of from 85 % or greater, or, from 90 % or greater, or, from 85 % to 95 %, or, from 88 to 94 %, or, 93.0 %.
35. The pectin of clause 33 having a galacturonic acid content (GalA) of from 75 % or less, or, from 70 % or less, or, from 65 % or less, or, from 60 % or less, or. from 50 to 75 %. or, from 55 to 65 %. or, from 57 to 61 %. or, 59.0 %.
36. The pectin of any one of clauses 33 to 35, wherein: the degree of esterification (DE) is from 18 to 40 %, or, from 20 to 35 %, or. from 23 to 31 %, or, from 23.3 to 31.0 %; the degree of amidation (DA) is from 12 to 25 %, or, from 15 to 23 %, or, from 16.0 to
22. 1 %; and/or wherein the degree of esterification (DE) to the degree of amidation (DA) is from 0.75 to 3.0, or, from 0.85 to 2.5, or. from 0.95 to 2.0. or, from 1.05 to 1.94.
37. The pectin of clause 33, clause 34 or clause 36, wherein: the degree of esterification (DE) is from 15 to 28 %; or, from 19 to 26 %, or, from 21 to 25 %, or, from 22 to 24 %, or, 23.3 %; the degree of amidation (DA) is from 5 to 30 %, or, from 10 to 25 %, or. 20 to 23 %, or.
22.1 %; and/or, the ratio of the degree of esterification (DE) to the degree of amidation (DA) is from 0.5 to 1.5, or, from 0.75 to 1.25, or, from 0.9 to 1.1, or. 1.05; wherein the pectin has a galacturonic acid content (GalA) of from galacturonic acid content (GalA) of from 85 % or greater, or, from 90 % or greater, or, from 85 % to 95 %, or, from 88 to 94 %, or, 93.0 %.
38. The pectin of clause 37, wherein; the degree of esterification (DE) is 23.3 % the degree of amidation (DA) is 22. 1 %, and the ratio of the degree of esterification (DE) to the degree of amidation (DA) is 1.05; and the galacturonic acid content (GalA) is 93.0 %.
39. The pectin of clause 37 or clause 38, wherein the pectin is sourced from citrus peel. 40. The pectin of clause 33. clause 35 or clause 36. wherein: the degree of esterification (DE) is from 25 to 35 %, or, from 30 to 32 %, or, 31.0 % the degree of amidation (DA) is from 10 to 20 %, or, 12.5 to 17.5 %, or, 16.0 %; the ratio of the degree of esterification (DE) to the degree of amidation (DA) is from 1.75 to 2.25, or, from 1.8 to 2.1, or, from 1.9 to 2.0, or, 1.94; and/or, wherein the pectin has a galacturonic acid content (Gal A) of from 75 % or less, or, from 70 % or less, or, from 65 % or less, or, from 60 % or less, or, from 50 to 75 %, or, from 55 to 65 %, or, from 57 to 61 %, or, 59.0 %.
41. The pectin of clause 40. wherein; the degree of esterification (DE) is 31.0 % the degree of amidation (DA) is 16.0 %, the ratio of the degree of esterification (DE) to the degree of amidation (DA) is 1.94; and the galacturonic acid content (GalA) is 59.0 %.
42. The pectin of clause 40 or clause 41, wherein the pectin is sourced from apple pomace.
43. The pectin of any one of clauses 33 to 42, wherein the degree of esterification (DE) is measured by titration; and/or. wherein the degree of amidation (DA) is measured by titration; and/or, wherein the galacturonic acid content (GalA) is measured by titration.
44. The pectin of any one of clauses 33 to 43, wherein the pectin is a low methoxyl (LM) amidated pectin, optionally wherein the low methoxyl amidated pectin has a degree of methylation of below 50 %.
45. Use of the pectin according to any one of clauses 33 to 44 in a food and/or beverage product; optionally, wherein the food and/or beverage product is a dairy product, a confectionary product, a reduced sugar jam product, fruit preparations and glazes.
46. A method of making a pectin according to any one of clauses 33 to 44, the method comprising the following steps: obtaining a high methoxyl (HM) pectin in aqueous form from a natural source; dry ing the high methoxyl (HM) pectin aqueous form to form a dry high methoxyl (HM) pectin, wherein the dry high methoxyl (HM) pectin has a moisture content of 10 weight % of the total weight of the dry7 high methoxyl (HM) pectin; placing the dry' high methoxyl (HM) pectin in a suspension comprising alcohol and ammonia to form an amidated low methoxyl (LM) pectin; and, dry ing the amidated low methoxyl (LM) pectin to form a pectin; optionally, the method further comprising any one or more of the following steps: clarifying the high methoxyl (HM) pectin in aqueous form; optionally wherein the high methoxyl (HM) pectin in aqueous form is clarified by centrifugation and/or filtration; concentrating the high methoxyl (HM) pectin in aqueous form; washing the high methoxyl (HM) pectin in aqueous form with alcohol; subjecting the high methoxyl (HM) pectin in aqueous form to a separation process; optionally, wherein the separation process is mechanical separation. filtering the amidated low methoxyl (LM) pectin; washing the amidated low methoxyl (LM) pectin with alcohol; and/or adjusting the pH of the amidated low methoxyl (LM) pectin.
47. A composition comprising: a pectin; and, water; wherein the pectin is the pectin of any one of clauses 33 to 44; optionally, wherein the composition further comprises sugar. optionally, wherein the sugar is any' one of sucrose, dextrose, lactose, maltose, glucose and/or galactose; optionally, wherein the sugar is present at from 20 to 60 weight %. or, from 30 to 50 weight %, or, from 35 to 45 weight %, or, at 40 weight % of the total weight of the composition.
48. Use of the composition according to clause 47, in a food and/or beverage product; optionally, wherein the food and/or beverage product is a dairy' product. 49. A method of making the composition of clause 47, the method comprising: providing a pectin; combining the pectin with water to form a composition; wherein the pectin is the pectin of any one of clauses 33 to 44; optionally, wherein the composition comprises the pectin at a concentration of from 0.001 to 10 weight % relative to the total amount of pectin and water, or, from 0.01 to 7.5 weight % relative to the total amount of pectin and water, or, from 0. 1 to 5 weight % relative to the total amount of pectin and water, or, from 0.2 to 3 weight % relative to the total amount of pectin and water, or, from 0.3 to 2.5 weight % relative to the total amount of pectin and water, or, from 0.4 to 2 weight % relative to the total amount of pectin and water.
BRIEF DESCRIPTION OF THE DRAWINGS
[00015] FIG. 1 is a flow diagram of a method for producing the pectin according to the present invention from dry HM pectin.
[00016] FIG. 2 is a plot of storage modulus (G’) and loss modulus (G”) for a composition comprising pectin and water according to the present invention (the composition analysed is Composition 1).
[00017] FIG. 3 is a plot of storage modulus (G’) versus concentration (C) for a composition comprising pectin and water according to the present invention (the composition analysed is Composition 1).
DETAILED DESCRIPTION
[00018] Embodiments of the invention are described below with reference to the accompanying drawings. The accompanying drawings illustrate various embodiments of systems, methods, and embodiments of various other aspects of the disclosure. Any person with ordinary skills in the art will appreciate that the illustrated element boundaries (e g., boxes, groups of boxes, or other shapes) in the figures represent one example of the boundaries. It may be that in some examples one element may be designed as multiple elements or that multiple elements may be designed as one element. In some examples, an element shown as an internal component of one element may be implemented as an external component in another and vice versa. Furthermore, elements may not be drawn to scale. Non-limiting and non-exhaustive descriptions are described with reference to the following drawings. The components in the figures are not necessarily to scale, emphasis instead being placed upon illustrating principles.
[00019] Embodiments of the present disclosure will be described more fully hereinafter with reference to the accompanying drawings in which like numerals represent like elements throughout the several figures, and in which example embodiments are shown. Embodiments of the claims may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein.
[00020] The words "comprising," "having," "containing," and "including," and other forms thereof, are intended to be equivalent in meaning and be open ended in that an item or items following any one of these words is not meant to be an exhaustive listing of such item or items or meant to be limited to only the listed item or items. Additionally, the phrase "‘consisting essentially of’ will be understood to include those elements specifically recited and those additionally elements that do not materially affect the basic and novel characteristics of the invention. The phrase “consisting of excludes any element not specified. It must also be noted that as used herein and in the appended claims, the singular forms "a," "an," and "the" include plural references unless the context clearly dictates otherwise. Although any systems and methods similar or equivalent to those described herein can be used in the practice or testing of embodiments of the present disclosure, the preferred systems and methods are now described.
[00021] As used herein, the terms “for example.” “for instance,” “such as,” or “including” are meant to introduce examples that further clarify more general subject matter. Unless otherwise specified, these examples are provided only as an aid for understanding the applications illustrated in the present disclosure and are not meant to be limiting in any fashion.
[00022] As used herein, “about” will be understood by persons of ordinary skill in the art and will vary to some extent depending upon the context in which it is used. If there are uses of the term which are not clear to persons of ordinary skill in the art, given the context in which it is used, “about” will mean up to plus or minus 10% of the particular term. [00023] In addition, it is to be understood that the phraseology or terminology employed herein, and not otherwise defined, is for the purpose of description only and not of limitation. Any use of section headings is intended to aid reading of the document and is not to be interpreted as limiting; information that is relevant to a section heading may occur within or outside of that particular section. In the event of inconsistent usages between this document and those documents so incorporated by reference, the usage in the incorporated reference should be considered supplementary to that of this document; for irreconcilable inconsistencies, the usage in this document controls.
[00024] Some of the terms used to describe the present invention are set out below:
[00025] “Amidation” refers to the modification of a pectin to include at least one amide group (-NH2).
[00026] “Critical gelling concentration” refers to the lowest concentration of a substance in a solvent, at which the substance is able to form a gel. A typical example is a composition comprising a pectin (i.e., the substance) in water (i.e., the solvent) with or without an additive (e.g., but not limited to sugars as defined herein below). The critical gelling concentration is dependent on molecular characteristics (such as, but not limited to, the degree of esterification (DE) and/or the degree of amidation (DA)) and environmental conditions (such as, but not limited to, the nature of the solvent, the ionic strength, the type of salts present and pH).
[00027] “Composition” refers to a mixture of at least two components. The mixture can be a solution, a suspension, or a dispersion.
[00028] “Degree of amidation” (DA) refers to the percentage of carboxyl groups that are amides. Theoretically, the degree of amide groups can range from 0 to 100 %. Preferably, the degree of amidation for a pectin is from 5 to 30 %. The degree of amidation can be measured by titration, an example of such method being given in EP 1517925. the disclosure of which is hereby incorporated by reference in its entirety.
[00029] “Degree of esterification” (DE) refers to the percentage of carboxyl groups that have undergone esterification. Theoretically, the degree of esterification can range from 0 to 100 %. The degree of esterification is also referred in the art as degree of methyl-esterification or degree of methylation (DM). The degree of esterification can be measured by titration, an example of such method being given in EP1294920 and EPl 171473, the disclosures of which are hereby incorporated by reference in their entirety.
[00030] “Degree of methylation” refers to the percentage of carboxyl groups esterified with methanol. If more than fifty percent of the carboxyl groups are methylated the pectin is called high methoxyl pectins (HM), and if less than that degree of methylation has occurred then the pectin is called low methoxyl pectins (LM).
[00031] “High methoxyl pectin” or “HM pectin” refers to a pectin extracted from the peels of citrus fruit, wherein a degree of the original carboxyl groups present in the pectin have undergone esterification with methanol. High methoxyl pectins have a degree of methylation of above 50 %.
[00032] “Low methoxyl pectin” or “LM pectin” refers to a pectin extracted from the peels of citrus fruit, wherein a degree of the original carboxyl groups present in the pectin have undergone esterification with methanol. Low methoxyl pectins have a degree of methylation of below 50 %.
[00033] “Homogeneous” refers to a substance with a uniform composition throughout. For example, a homogeneous substance does not present gradients of a certain property (e.g., concentration) larger than 1 weight % of the calculated property. According to this invention, the composition may comprise a pectin, wherein the pectin is homogeneous (i.e., the composition comprises only one type of pectin). By one type of pectin is herein understood that the pectin used in accordance with the invention is obtained from a single source of pectin and has a certain degree of amidation and a certain degree of esterification.
[00034] “Low methoxyl amidated pectin” or “LM amidated pectin” or “LMA pectin” refers to a modified form of LM pectin in which some or at least some of the methoxyl groups are converted by ammonia into carboxylic amides. Preferably, LM amidated pectins have a degree of amidation of from 5 and 30 %. [00035] “Mix” or “mixture” refers to a substance containing two or more different components, whereas the term “mixed” refers to a method step wherein a mix or mixture is formed.
[00036] “Pectin” refers to an anionic water-soluble plant cell wall polysaccharide comprising a chain of galacturonic acid units which are linked by a-1,4 glycosidic bonds. The galacturonic acid chain is partly esterified, i.e.. the galacturonic chain contains methyl ester groups. Other chemicals such as acetyl can be incorporated into the galacturonic acid chain and can be important for distinguishing between different pectin types.
[00037] “Pectin gel” refers to a sample containing a three-dimensional (3-D) network of pectin molecules. A pectin gel is the result of the association of long stretches of pectin polymer chain into conformationally ordered junction zones that are stabilised by arrays of noncovalent interactions. Pectin gels possess both the viscous properties of liquids and the elastic properties of solids, i.e., they are viscoelastic materials. Pectin gels have been known to the skilled person for decades, e.g. from M.A.V. Axelos et al. "CHAPTER 11 - Rheology of Pectin Dispersions and Gels”, The Chemistry and Technology of Pectin, Food Science and Technology, 1991, Pages 227-250, ISBN 978-0-08-092644-5, the disclosure of which is hereby incorporated by reference in its entirety.
[00038] “Temperature of gelation” (Tg) refers to the temperature at which a material undergoes reverse thermal gelation, i.e., the temperature below which the material is soluble in water and above which the material undergoes phase transition to increase in viscosity or to form a serni-solid gel. For example, for gelling polysaccharides such as pectins, gelation temperature (Tg) refers to the temperature at which a solution containing pectin transitions from a liquid state to a gel.
Composition
[00039] Compositions according to the presently described invention have various desirable properties, which make these compositions useful for utilisation in various food and beverage products.
Composition: Temperature of gelation [00040] The composition comprises a pectin and water.
[00041] The pectin is present in the composition in an amount of from 0.001 to 10 weight % relative to the total amount of pectin and water, preferably from 0.01 to 7.5 weight % relative to the total amount of pectin and water, more preferably from 0. 1 to 5 weight % relative to the total amount of pectin and water, even more preferably from 0.2 to 3 weight % relative to the total amount of pectin and water, even more preferably from 0.3 to 2.5 weight % relative to the total amount of pectin and water, most preferably from 0.4 to 2 weight % relative to the total amount of pectin and water.
[00042] The composition has a temperature of gelation (Tg), wherein when the concentration of the pectin relative to the total amount of pectin and water is increased from 0.8 weight % to 1.4 weight %, the temperature of gelation (Tg) varies by from 0.5 to 2.5 °C, preferably from 0.5 to 2.0 °C. more preferably from 0.75 to 1.5 °C, even more preferably from 1.0 to 1.3 °C, most preferably from 1.03 to 1.27 °C. Preferably, when the concentration of the pectin in the water is increased from 0.8 weight % to 1.4 weight % relative to the total amount of pectin and water, the temperature of gelation (Tg) varies by from 1.03 to 1.27°C.
[00043] The pectin in the composition preferably has a degree of esterification (DE) of from 15 to 45 %, more preferably from 18 to 40 %, even more preferably from 20 to 35 %, even more preferably from 23 to 31 %, most preferably from 23.3 to 31.0 %.
[00044] The pectin in the composition has a degree of amidation (DA) of from 5 to 30 %, more preferably from 12 to 25 %, even more preferably from 15 to 23 %, most preferably from 16.0 to 22.1 %.
[00045] The pectin in the composition may have a ratio of a degree of esterification (DE) to a degree of amidation (DA) of from 0.75 to 3.0, preferably from 0.85 to 2.5, more preferably from 0.95 to 2.0, most preferably from 1.05 to 1.94.
[00046] Preferably, the pectin in the composition has a degree of esterification (DE) of from 15 to 45 %, more preferably from 18 to 40 %, even more preferably from 20 to 35 %, even more preferably from 23 to 31 %, most preferably from 23.3 to 31.0 %; a degree of amidation (DA) of from 5 to 30 %, more preferably from 12 to 25 %, even more preferably from 15 to 23 %. most preferably from 16.0 to 22. 1 %, and. a ratio of a degree of esterification (DE) to a degree of amidation (DA) of from 0.75 to 3.0, preferably from 0.85 to 2.5, more preferably from 0.95 to 2.0, most preferably from 1.05 to 1.94. More preferably, the pectin in the composition has a degree of esterification (DE) of from 23.3 to 31 %, a degree of amidation (DA) of from 16.0 to 22. 1 %, and. a ratio of a degree of esterification (DE) to a degree of amidation (DA) of from 1.05 to 1.94.
[00047] The pectin may be sourced from any one of apples, apple pomace, citrus fruits, citrus peel, lemons, mandarin oranges, grapefruit, sweet orange, pomelo, clementines, limes, kumquat, bitter oranges, blood oranges, satsumas, yuzus. tangelos, or, any combinations thereof.
[00048] The composition may comprise apple pectin, for example pectin extracted from apple pomace. The composition may comprise apple pectin and water, and when the pectin concentration in the water is increased from 0.8 weight % to 1.4 weight % relative to the total amount of pectin and water, the temperature of gelation is 1.27°C. Preferably, said pectin also has a ratio of a degree of esterification (DE) to a degree of amidation (DA) of from 1.9 to 2.0, preferably, 1.94. Preferably, the entire amount of pectin present in the composition is apple pectin.
[00049] The composition may comprise citrus pectin, for example pectin extracted from citrus fruits, e.g., citrus peel. The composition may comprise citrus pectin and water, and when the pectin concentration in the water is increased from 0.8 weight % to 1.4 weight % relative to the total amount of pectin and water, the temperature of gelation is 1.03 °C. Preferably, wherein the pectin also has a ratio of a degree of esterification (DE) to a degree of amidation (DA) of from 1.00 to 1.10, preferably 1.05. Preferably, the entire amount of pectin present in the composition is citrus pectin.
[00050] The degree of esterification and the degree of amidation may be measured by titration techniques.
[00051] The pectin in the composition may be homogeneous. [00052] The composition comprises pectin and water, wherein the pectin is preferably extracted from a single pectin source, said pectin source being chosen from the group consisting of apples, apple pomace, citrus fruits, citrus peel, lemons, mandarin oranges, grapefruit, sweet orange, pomelo, clementines, limes, kumquat, bitter oranges, blood oranges, satsumas, yuzus, tangelos, or, any combinations thereof.
[00053] Preferably, the composition consists of a pectin and water, preferably, wherein the pectin is homogeneously distributed inside the water.
[00054] The pectin in the composition may be amidated. Preferably, the pectin in the composition may be a LM amidated pectin.
[00055] The composition may comprise sugar. The sugar may be, but is not necessarily limited to, sucrose, dextrose, lactose, maltose, glucose and/or galactose. Preferably, the sugar is sucrose. Preferably, the composition comprises the sugar at from 20 to 60 weight %, more preferably from 30 to 50 weight %. even more preferably from 35 to 45 weight %, most preferably at 40 weight % of the total weight of the composition.
[00056] The composition may additionally comprise a gel-promoting medium and/or a buffer.
[00057] Preferably, wherein the gel-promoting medium comprises citric acid monohydrate, tri-sodium citrate dihydrate, sodium benzoate, calcium chloride dihydrate and water. Preferably, wherein the citric acid monohydrate is present at from 300 to 350 g, more preferably at from 320 to 330 g, most preferably at 325.598 g. Preferably, wherein the trisodium citrate dihydrate is present at from 150 to 200 g, more preferably from 160 to 170 g, most preferably at 167.493 g. Preferably, wherein the sodium benzoate is present at from 0.5 to 10 g, more preferably from 3 to 7 g, most preferably at 5 g. Preferably, wherein the calcium chloride dihydrate is present at from 0.5 to 10 g, more preferably from 4 to 8 g, most preferably at 6.2 g. Preferably, wherein the distilled water is present at from 4000 to 5000 g, more preferably, at from 4400 to 4600 g, most preferably at 4495.709 g. Preferably, wherein the citric acid monohydrate is present at 325.598 g, the tri-sodium citrate dihydrate is present at 167.493 g, the sodium benzoate is present at 5 g, the calcium chloride dihydrate is present at 6.2 g and the distilled water is present at 4495.709 g. [00058] Preferably, wherein the buffer comprises sodium citrate and water. Preferably, the buffer contains sodium citrate so that the pH of the buffer is from 3 to 4, more preferably from 3.2 to 3.6, most preferably 3.4.
[00059] Preferably, the composition has a temperature of gelation (Tg) wherein when the concentration of the pectin relative to the total amount of pectin and water is increased from 0.8 weight % to 1 .4 weight %, the temperature of gelation (Tg) varies by from 0.5 to 2.5°C; and wherein the composition further comprises a gel-promoting medium and a buffer; wherein the gel-promoting medium comprises citric acid monohydrate, tri-sodium citrate dihydrate, sodium benzoate, calcium chloride dihydrate and water; and wherein the buffer comprises sodium citrate and water.
Composition: Critical gelling concentration
[00060] The composition comprises a pectin and water.
[00061] The pectin is present in the composition in an amount of from 0.001 to 10 weight % relative to the total amount of pectin and water, preferably from 0.01 to 7.5 weight % relative to the total amount of pectin and water, more preferably from 0. 1 to 5 weight % relative to the total amount of pectin and water, even more preferably from 0.2 to 3 weight % relative to the total amount of pectin and water, even more preferably from 0.3 to 2.5 weight % relative to the total amount of pectin and water, most preferably from 0.4 to 2 weight % relative to the total amount of pectin and water.
[00062] The composition has a critical gelling concentration (Co) of from 0.01 to 0.2 weight %, preferably from 0.02 to 0.17 weight %, more preferably from 0.025 to 0.15 weight %, even more preferably from 0.04 to 0. 13 weight %, most preferably from 0.05 to 0. 12 weight %.
[00063] The pectin in the composition preferably has a degree of esterification (DE) of from 15 to 45 %, more preferably from 18 to 40 %, even more preferably from 20 to 35 %, even more preferably from 23 to 31 %. most preferably from 23.3 to 31.0 %. [00064] The pectin in the composition has a degree of amidation (DA) of from 5 to 30 %, more preferably from 12 to 25 %. even more preferably from 15 to 23 %, most preferably from 16.0 to 22.1 %.
[00065] The pectin in the composition may have a ratio of a degree of esterification (DE) to a degree of amidation (DA) of from 0.75 to 3.0, preferably from 0.85 to 2.5, more preferably from 0.95 to 2.0, even most preferably from 1.05 to 1.94.
[00066] Preferably, the pectin in the composition has a degree of esterification (DE) of from 15 to 45 %, more preferably from 18 to 40 %, even more preferably from 20 to 35 %, even more preferably from 23 to 31 %. most preferably from 23.3 to 31.0 %; a degree of amidation (DA) of from 5 to 30 %, more preferably from 12 to 25 %, even more preferably from 15 to 23 %, most preferably from 22. 1 to 16.0 %, and, a ratio of a degree of esterification (DE) to a degree of amidation (DA) of from 0.75 to 3.0, preferably from 0.85 to 2.5, more preferably from 0.95 to 2.0, most preferably from 1.05 to 1.94. More preferably, the pectin in the composition has a degree of esterification (DE) of from 23.3 to 31 %. a degree of amidation (DA) of from 16.0 to 22. 1 %, and, a ratio of a degree of esterification (DE) to a degree of amidation (DA) of from 1.05 to 1.94.
[00067] Preferably, the composition may comprise a pectin and water, wherein the critical gelling concentration (Co) is from 0.05 to 0.12 weight %, and preferably wherein the pectin has a ratio of a degree of esterification (DE) to a degree of amidation (DA) of from 1.05 to 1.94.
[00068] The pectin may be sourced from any one of apples, apple pomace, citrus fruits, citrus peel, lemons, mandarin oranges, grapefruit, sweet orange, pomelo, clementines, limes, kumquat, bitter oranges, blood oranges, satsumas, yuzus, tangelos, or, any combinations thereof.
[00069] The composition may comprise apple pectin, for example pectin extracted from apple pomace. The composition may comprise apple pectin and water, wherein the critical gelling concentration (Co) is 0. 12 weight %, and preferably wherein the pectin has a ratio of a degree of esterification (DE) to a degree of amidation (DA) of from 1.94. Preferably, the entire amount of pectin present in the composition is apple pectin. [00070] The composition may comprise citrus pectin, for example pectin extracted from citrus fruits, e.g., citrus peel. The composition may comprise citrus pectin and water, wherein the critical gelling concentration (Co) is 0.05 weight %, and preferably wherein the pectin has a ratio of a degree of esterification (DE) to a degree of amidation (DA) of 1.05. Preferably, the entire amount of pectin present in the composition is citrus pectin.
[00071] The degree of esterification and the degree of amidation may be measured by titration techniques.
[00072] The pectin in the composition may be homogeneous.
[00073] The composition comprises pectin and water, wherein the pectin is preferably extracted from a single pectin source, said pectin source being chosen from the group consisting of apples, apple pomace, citrus fruits, citrus peel, lemons, mandarin oranges, grapefruit, sweet orange, pomelo, clementines, limes, kumquat, bitter oranges, blood oranges, satsumas, yuzus. tangelos, or. any combinations thereof.
[00074] Preferably, the composition consists of a pectin and water, preferably, wherein the pectin is homogeneously distributed inside the water.
[00075] The pectin in the composition may be amidated. Preferably, the pectin in the composition may be a LM amidated pectin.
[00076] The composition may comprise sugar. The sugar may be. but is not necessarily limited to, sucrose, dextrose, lactose, maltose, glucose and/or galactose. Preferably, the sugar is sucrose. Preferably, the composition comprises the sugar at from 20 to 60 weight %, preferably from 30 to 50 weight %, more preferably from 35 to 45 weight %, most preferably at 40 weight % of the total weight of the composition.
[00077] The composition may additionally comprise a gel-promoting medium and/or a buffer.
[00078] Preferably, wherein the gel -promoting medium comprises citric acid monohydrate, tri-sodium citrate dihydrate, sodium benzoate, calcium chloride dihydrate and water. Preferably, wherein the citric acid monohydrate is present at from 300 to 350 g, more preferably at from 320 to 330 g, most preferably at 325.598 g. Preferably, wherein the trisodium citrate dihydrate is present at from 150 to 200 g, more preferably from 160 to 170 g, most preferably at 167.493 g. Preferably, wherein the sodium benzoate is present at from 0.5 to 10 g, more preferably from 3 to 7 g, most preferably at 5 g. Preferably, wherein the calcium chloride dihydrate is present at from 0.5 to 10 g, more preferably from 4 to 8 g, most preferably at 6.2 g. Preferably, wherein the distilled water is present at from 4000 to 5000 g, more preferably, at from 4400 to 4600 g, most preferably at 4495.709 g. Preferably, wherein the citric acid monohydrate is present at 325.598 g, the tri-sodium citrate dihydrate is present at 167.493 g, the sodium benzoate is present at 5 g, the calcium chloride dihydrate is present at 6.2 g and the distilled water is present at 4495.709 g.
[00079] Preferably, wherein the buffer comprises sodium citrate and water, Preferably, the buffer contains sufficient sodium citrate so that the pH of the buffer is from 3 to 4. more preferably from 3.2 to 3.6, most preferably 3.4.
[00080] Preferably, the composition has a critical gelling concentration (Co) wherein the critical gelling concentration (Co) varies by from 0.01 to 0.2 weight %, wherein the composition further comprises a gel-promoting medium and a buffer; wherein the gel-promoting medium comprises citric acid monohydrate, tri-sodium citrate dihydrate, sodium benzoate, calcium chloride dihydrate and water; and wherein the buffer comprises sodium citrate and water.
Composition: Temperature of gelation and critical gelling concentration
[00081] The composition comprises a pectin and water.
[00082] The pectin is present in the composition in an amount of from 0.001 to 10 weight % relative to the total amount of pectin and water, preferably from 0.01 to 7.5 weight % relative to the total amount of pectin and water, more preferably from 0. 1 to 5 weight % relative to the total amount of pectin and water, even more preferably from 0.2 to 3 weight % relative to the total amount of pectin and water, even more preferably from 0.3 to 2.5 weight % relative to the total amount of pectin and water, most preferably from 0.4 to 2 weight % relative to the total amount of pectin and water. [00083] The composition has a temperature of gelation (Tg) and a critical gelling concentration (Co), wherein when the concentration of the pectin relative to the total amount of pectin and water is increased from 0.8 weight % to 1.4 weight %, the temperature of gelation (Tg) varies by from 0.5 to 2.5°C preferably from 0.5 to 2.0 °C, more preferably from 0.75 to 1.5 °C, even more preferably from 1.0 to 1.3 °C, most preferably from 1.03 to 1.27 °C, and, wherein the critical gelling concentration (Co) is from 0.01 to 0.2 weight %, preferably from 0.02 to 0.17 weight %. more preferably from 0.025 to 0. 15 weight %. even more preferably from 0.04 to 0. 13 weight %, most preferably from 0.05 to 0. 12 weight %.
[00084] Preferably, the composition may have a temperature of gelation (Tg) and a critical gelling concentration (Co), wherein when the concentration of the pectin relative to the total amount of pectin and water is increased from 0.8 weight % to 1.4 weight %, the temperature of gelation (Tg) varies by from 1.03 to 1.27 °C, and, wherein the critical gelling concentration (Co) is from 0.05 to 0.12 weight %.
[00085] The pectin in the composition preferably has a degree of esterification (DE) of from 15 to 45 %, more preferably from 18 to 40 %, even more preferably from 20 to 35 %, even more preferably from 23 to 31 %, most preferably from 23.3 to 31.0 %.
[00086] The pectin in the composition has a degree of amidation (DA) of from 5 to 30 %, more preferably from 12 to 25 %, even more preferably from 15 to 23 %, most preferably 16.0 to 22.1 %.
[00087] The pectin in the composition may have a ratio of a degree of esterification (DE) to a degree of amidation (DA) of from 0.75 to 3.0, preferably from 0.85 to 2.5, more preferably from 0.95 to 2.0, even most preferably from 1.05 to 1.94.
[00088] Preferably, the pectin in the composition has a degree of esterification (DE) of from 15 to 45 %, more preferably from 18 to 40 %, even more preferably from 20 to 35 %, even more preferably from 23 to 31 %, most preferably from 23.3 to 31.0 %; a degree of amidation (DA) of from 5 to 30 %, more preferably from 12 to 25 %, even more preferably from 15 to 23 %. most preferably from 16.0 to 22. 1 %, and. a ratio of a degree of esterification (DE) to a degree of amidation (DA) of from 0.75 to 3.0, preferably from 0.85 to 2.5. more preferably from 0.95 to 2.0, most preferably from 1.05 to 1.94. More preferably, the pectin in the composition has a degree of esterification (DE) of from 23.3 to 31 %, a degree of amidation (DA) of from 16.0 to 22. 1 %, and. a ratio of a degree of esterification (DE) to a degree of amidation (DA) of from 1.05 to 1.94.
[00089] The pectin may be sourced from any one of apples, apple pomace, citrus fruits, citrus peel, lemons, mandarin oranges, grapefruit, sweet orange, pomelo, clementines, limes, kumquat, bitter oranges, blood oranges, satsumas, yuzus. tangelos, or. any combinations thereof.
[00090] The degree of esterification and the degree of amidation may be measured by titration techniques.
[00091] The pectin in the composition may be homogeneous.
[00092] The composition comprises pectin and water, wherein the pectin is preferably extracted from a single pectin source, said pectin source being chosen from the group consisting of apples, apple pomace, citrus fruits, citrus peel, lemons, mandarin oranges, grapefruit, sweet orange, pomelo, clementines, limes, kumquat, bitter oranges, blood oranges, satsumas, yuzus, tangelos, or, any combinations thereof.
[00093] Preferably, the composition consists of a pectin and water, preferably, wherein the pectin is homogeneously distributed inside the water.
[00094] The pectin in the composition may be amidated. Preferably, the pectin in the composition may be a LM amidated pectin.
[00095] The composition may comprise sugar. The sugar may be, but is not necessarily limited to, sucrose, dextrose, lactose, maltose, glucose and/or galactose. Preferably, the sugar is sucrose. Preferably, the composition comprises the sugar at from 20 to 60 weight %, preferably from 30 to 50 weight %, more preferably from 35 to 45 weight %. most preferably at 40 weight % of the total weight of the composition.
[00096] The composition may additionally comprise a gel-promoting medium and/or a buffer. [00097] Preferably, wherein the gel-promoting medium comprises citric acid monohydrate, tri-sodium citrate dihydrate, sodium benzoate, calcium chloride dihydrate and water. Preferably, wherein the citric acid monohydrate is present at from 300 to 350 g, more preferably at from 320 to 330 g, most preferably at 325.598 g. Preferably, wherein the trisodium citrate dihydrate is present at from 150 to 200 g, more preferably from 160 to 170 g, most preferably at 167.493 g. Preferably, wherein the sodium benzoate is present at from 0.5 to 10 g, more preferably from 3 to 7 g, most preferably at 5 g. Preferably, wherein the calcium chloride dihydrate is present at from 0.5 to 10 g, more preferably from 4 to 8 g, most preferably at 6.2 g. Preferably, wherein the distilled water is present at from 4000 to 5000 g, more preferably, at from 4400 to 4600 g, most preferably at 4495.709 g. Preferably, wherein the citric acid monohydrate is present at 325.598 g, the tri-sodium citrate dihydrate is present at 167.493 g, the sodium benzoate is present at 5 g, the calcium chloride dihydrate is present at 6.2 g and the distilled water is present at 4495.709 g.
[00098] Preferably, wherein the buffer comprises sodium citrate and water, Preferably, the buffer contains sufficient sodium citrate so that the pH of the buffer is from 3 to 4. more preferably from 3.2 to 3.6, most preferably 3.4.
[00099] Preferably, the composition has a temperature of gelation (Tg) and a critical gelling concentration (Co), wherein when the concentration of the pectin relative to the total amount of pectin and water is increased from 0.8 weight % to 1 .4 weight %, the temperature of gelation (Tg) varies by from 0.5 to 2.5°C; wherein the critical gelling concentration (Co) is from 0.01 to 0.2 weight %; wherein the composition further comprises a gel-promoting medium and a buffer; wherein the gel-promoting medium comprises citric acid monohydrate, tri-sodium citrate dihydrate, sodium benzoate, calcium chloride dihydrate and water; and wherein the buffer comprises sodium citrate and water.
The composition as a pectin gel
[000100] The composition as set out under the heading “Composition” can be in the form of a pectin gel. Pectin gels according to the presently described invention have various desirable properties, which make these pectin gels useful in various food and beverage products. [000101] The pectin gel comprises the composition as set out under the heading "Composition", i.e.. the pectin gel comprises water and pectin.
[000102] The pectin is present in the pectin gel in an amount of from 0.001 to 10 weight % relative to the total amount of pectin gel, preferably from 0.01 to 7.5 weight % relative to the total amount of pectin gel, more preferably from 0. 1 to 5 weight % relative to the total amount of pectin gel, even more preferably from 0.2 to 3 weight % relative to the total amount of pectin gel, even more preferably from 0.3 to 2.5 weight % relative to the total amount of pectin gel, most preferably from 0.4 to 2 weight % relative to the total amount of pectin gel.
[000103] The pectin gel may further comprise an additional material which is, but not limited to, sucrose, glucose, fructose, ribose, glyceraldehyde, lactose, maltose, glycerol, erythritol, sorbitol, xylitol, mannitol, lactitol, maltitol, or any combinations thereof. Preferably, the pectin gel comprises the additional material at from 20 to 60 weight %, preferably from 30 to 50 weight %, more preferably from 35 to 45 weight %, most preferably at 40 weight % of the total weight of the pectin gel.
[000104] The pectin gel may further comprise fragrants, flavourants, colourants, preservatives and the like. The pectin gel may comprise gel-promoting mediums, such as but not limited to calcium.
[000105] The pectin gel may comprise one or more immiscible materials dispersed throughout the pectin gel. Preferably, the water immiscible material is dispersed in the gel in the form of an emulsion. Preferably, the water immiscible material is a volatile organic component such as an oil, or, an organic oil immiscible in water, or, an aqueous matrix. Preferably, the water immiscible material is, but not limited to, perfume, flavourant, pheromone, bactericide, insect attractant, insect repellent, animal attractant, animal repellent, insecticide, fungicide, pharmaceutical drug, veterinary drug, other volatile oils or organic materials, or any combinations thereof.
Method of making the pectin [000106] Another aspect of the present invention relates to the method of making a pectin. In particular, this aspect of the present invention relates to a method of making a LM amidated pectin.
[000107] In the method of making the pectin, HM pectin is first extracted from citrus peel or apple pomace. The extracted HM pectin then undergoes amidation to form a LM amidated pectin.
[000108] FIG. 1 depicts a flow diagram for method 1.
[000109] Step 1: Extraction of HM pectin from a natural source of pectin
[000110] First, a natural source of pectin is mixed in acidic, hot water to extract the HM pectin from the natural source of pectin in aqueous form following the methodology described elsewhere such as in Endreb, H.-U., & Christensen, S. H. (2020). Pectins. In G. O. Philips & P. A. Williams (Eds.). Handbook of hydrocolloids (3rd ed.. pp. 274-297). Cambridge: Woodhead Publishing Limited, the disclosure of which is hereby incorporated by reference in its entirety. Typically, the natural source of pectin is a raw material extracted from fruit.
[000111] In this method, the natural source of pectin can be fruits such as apples, apple pomace, pears, plums, guavas, quince, gooseberries and citrus fruits such as citrus peel, lemons, mandarin oranges, grapefruit, sweet orange, pomelo, clementines, limes, kumquat, bitter oranges, blood oranges, satsumas, yuzus, tangelos, or, any combinations thereof. Preferably, the fruit extract is sourced from apple pomace and/or citrus peel.
[000112] Preferably, the temperature of the acidic, hot water is from 60 to 80°C, or, from 65 to 75°C, or, from 68 to 72°C.
[000113] Preferably, the pH of the acidic, hot water is from pH 1 to 2, or, from pH 1.25 to 1.95, or, from pH 1.4 to 1.8, or, from pH 1.45 to 1.75, or, from pH 1.50 to 1.70.
[000114] Preferably, the residence time of the fruit extract in the acidic, hot water is from 1 to 20 hours, or, from 6 to 14 hours, or, from 7 to 13 hours, or, from 8 to 12 hours. [000115] Preferably, the temperature of the acidic, hot water is from 68 to 72°C, the pH of the acidic, hot water is from pH 1.50 to 1.70 and the residence time of the fruit extract in the acidic, hot water is from 8 to 12 hours.
[000116] The HM pectin in aqueous form may then be clarified by using centrifugation, filtration or other conventional separation technologies known in the art to obtain a clarified HM pectin in aqueous form.
[000117] The clarified HM pectin in aqueous form may then be concentrated to form a concentrated HM pectin in aqueous form by using any technique known in the art.
[000118] An alcohol may be added to the concentrated HM pectin in aqueous form to cause the HM extract to precipitate out as a precipitate containing the HM pectin. The amount of alcohol added depends on the amount of alcohol required to cause the clarified HM extract to precipitate out from its aqueous form as a precipitate containing the HM pectin.
[000119] Preferably, the alcohol used is one or more of isopropanol, tert-amyl alcohol, benzy l alcohol , 1,4-butanediol, 1, 2, 4-butanetriol, butanol, 1 -butanol, 2-butanol, tert-butyl alcohol, diethylene glycol, ethanol, ethylene glycol, 2-ethylhexanol, furfuryl alcohol, glycerol, iso-butanol, isopropyl alcohol, methanol. 2-(2-methoxyethoxyl)ethanol, 2-methyl-l -butanol, 2- methyl-1 -pentanol, 3-methyl-2-butanol, neopentyl alcohol, 2-pentanol, 1,3-propanedioL propan- l-ol, propylene glycol, propylene glycol methyl ether, or, any combination thereof. Preferably, the alcohol is isopropyl alcohol.
[000120] The precipitate containing the HM pectin may be separated from the alcohol/ water mix. Preferably, the precipitate containing the HM pectin is separated from the alcohol/ water mix by mechanical separation, wherein any mechanical separation known in the art can be used.
[000121] The precipitate containing the HM pectin obtained from the separation is washed with alcohol to form a washed precipitate containing the HM pectin.
[000122] Preferably, the alcohol used is one or more of isopropanol, tert-amyl alcohol, benzyl alcohol , 1,4-butanediol, 1, 2, 4-butanetriol, butanol, 1 -butanol, 2-butanol, tert-butyl alcohol, diethylene glycol, ethanol, ethylene glycol, 2-ethylhexanol, furfuryl alcohol, glycerol, iso-butanol, isopropyl alcohol, methanol. 2-(2-methoxyethoxyl)ethanol, 2 -methyl- 1 -butanol, 2- methyl-1 -pentanol, 3-methyl-2-butanol, neopentyl alcohol, 2-pentanol, 1,3 -propanediol, propan- l-ol, propylene glycol, propylene glycol methyl ether, or, any combination thereof. Preferably, the alcohol is isopropyl alcohol.
[000123] Preferably, the precipitate containing the HM amidated pectin obtained from the separation is washed with the alcohol one, two, three, four, five, six, seven, eight, nine, ten, or more than ten times. Preferably, the HM amidated pectin is washed with the alcohol three times.
[000124] Preferably, the precipitate containing the HM amidated pectin obtained from the separation is washed with alcohol at from 50 to 70 weight %, or, from 55 to 65 weight %, or, at 60 weight % of the total weight of the alcohol to form a washed HM pectin.
[000125] Preferably, the alcohol used is one or more of isopropanol, tert-amyl alcohol, benzyl alcohol . 1,4-butanediol. 1, 2, 4-butanetrioL butanol, 1 -butanol. 2-butanol, tert-butyl alcohol, diethylene glycol, ethanol, ethylene glycol, 2-ethylhexanol, furfuryl alcohol, glycerol, iso-butanol, isopropyl alcohol, methanol, 2-(2-methoxy ethoxy l)ethanol, 2 -methyl- 1 -butanol, 2- methyl-1 -pentanol, 3-methyl-2-butanol, neopentyl alcohol. 2-pentanol, 1,3-propanediol. propan- l-ol. propylene glycol, propylene glycol methyl ether, or, any combination thereof. Preferably, the alcohol is isopropyl alcohol.
[000126] The washed HM pectin may then undergo a drying step to form a dry HM pectin. The drying step dries the washed HM pectin until the washed HM pectin has a moisture content of from 5 to 15 weight %, or, from 7.5 to 12.5 weight %, or, 10 weight % of the total weight of the dry HM pectin. Preferably, the drying step is carried out by press-drying. The product of the dry ing step is a dry HM pectin.
[000127] The dry HM pectin can be ground until a homogeneous particle size distribution is achieved. The dry HM pectin can be blended with sugar to form a standardised HM pectin.
[000128] For the product of the first step to be the pectin of the present invention, parameters of the above process need to be tightly controlled. Step 2: Amidation of dry HM pectin
[000129] The dry HM pectin may be placed in a suspension which comprises alcohol and ammonia to form an amidated LM pectin.
[000130] Preferably, the alcohol used is one or more of isopropanol, tert-amyl alcohol, benzyl alcohol . 1,4-butanediol. 1, 2, 4-butanetriol. butanol, 1 -butanol. 2-butanol, tert-butyl alcohol, diethylene glycol, ethanol, ethylene glycol, 2-ethylhexanol, furfuryl alcohol, glycerol, iso-butanol, isopropyl alcohol, methanol, 2-(2-methoxy ethoxy l)ethanol, 2 -methyl- 1 -butanol, 2- methyl-1 -pentanol, 3-methyl-2-butanol, neopentyl alcohol. 2-pentanol, 1,3-propanediol. propan- l-ol. propylene glycol, propylene glycol methyl ether, or, any combination thereof. Preferably, the alcohol is isopropyl alcohol.
[000131] Preferably, the alcohol is present at from 50 to 80 weight %, or, from 55 to 75 weight %, or, from 60 to 70 weight % of the total weight of the suspension. Preferably, the alcohol is present at from 60 to 70 weight % of the total weight of the suspension.
[000132] Preferably, the ammonia is present at from 2 to 4 weight %, or, from 2.5 to 3.75 weight %, or, from 2.8 to 3.5 weight % of the total weight of the suspension. Preferably, the ammonia is present at from 2.8 to 3.5 weight % of the total weight of the suspension.
[000133] Preferably, the suspension is maintained at a temperature of from 5 to 20 °C, or, from 8 to 16 °C , or, from 9 to 15 °C, or, from 10 to 14 °C. Preferably, the suspension is maintained at a temperature of from 10 to 14 °C.
[000134] Preferably, the dry7 HM pectin is maintained in the suspension for from 3 to 10 hours, or, from 4 to 9 hours, or, from 5 to 8 hours. Preferably, the dry HM pectin is maintained in the suspension for from 5 to 8 hours.
[000135] Preferably, the alcohol is present at from 60 to 70 weight % of the total weight of the suspension, the ammonia is present at from 2.8 to 3.5 weight % of the total weight of the suspension, the suspension is maintained at a temperature of from 10 to 14 °C, the dry HM pectin is maintained in the suspension for from 5 to 8 hours and the alcohol used is isopropyl alcohol. [000136] The LM amidated pectin can be filtered out of the suspension to produce a filtrate comprising the alcohol and a residue comprising the LM amidated pectin. The LM amidated pectin can be filtered out of the suspension by any filtration technique known in the art.
[000137] Preferably, the filtrate comprising the alcohol and ammonia pass to a recovery step.
[000138] Preferably, the residue comprising the LM amidated pectin can be washed to form a w ashed LM amidated pectin. Preferably, the residue comprising the LM amidated pectin is washed with alcohol. Preferably, the residue comprising the LM amidated pectin is washed with alcohol at from 50 to 70 weight %, or, from 55 to 65 weight %, or, at 60 weight % of the total weight of the alcohol. Preferably, the alcohol used is isopropyl alcohol. Preferably, the alcohol used is one or more of isopropanol, tert-amyl alcohol, benzyl alcohol , 1,4-butanediol, 1, 2, 4-butanetriol. butanol, 1 -butanol. 2-butanol, tert-butyl alcohol, di ethylene glycol, ethanol, ethylene glycol. 2-ethylhexanol, furfuryl alcohol, glycerol, iso-butanol, isopropyl alcohol, methanol, 2-(2-methoxyethoxyl)ethanol, 2-methyl-l -butanol, 2-methy 1-1 -pentanol, 3-methyl-2- butanol, neopentyl alcohol, 2-pentanol, 1,3-propanediol, propan-l-ol, propylene glycol, propylene glycol methyl ether, or, any combination thereof. Preferably, the alcohol is isopropyl alcohol.
[000139] Preferably, the pH of the washed LM amidated pectin can be adjusted until the pH lies from 3.0 to 5.5, or, from 3.5 to 4.0, or, from 4.0 to 4.5.
[000140] Preferably, the pH of the washed LM amidated pectin is adjusted with acid to form a pH adjusted LM amidated pectin. Preferably, the acid is nitric acid.
[000141] The pH adjusted LM amidated pectin may be washed with alcohol to form a second-washed LM amidated pectin.
[000142] Preferably, the alcohol is any one of tert-amyl alcohol, benzy l alcohol , 1,4- butanediol, 1, 2, 4-butanetriol, butanol, 1 -butanol, 2-butanol, tert-butyl alcohol, diethylene glycol, ethanol, ethylene glycol, 2-ethylhexanol, furfuryl alcohol, glycerol, iso-butanol, isopropyl alcohol, methanol, 2-(2-methoxyethoxyl)ethanol, 2-methyl-l -butanol, 2-methyl-l- pentanol, 3-methyl-2-butanol, neopentyl alcohol, 2-pentanol, 1,3-propanediol, propan-l-ol, propylene glycol, propylene glycol methyl ether, isopropanol, or, any combination thereof. Preferably, the alcohol is isopropyl alcohol.
[000143] Preferably, the neutralised LM ami dated pectin is washed with the alcohol one, two, three, four, five, six, seven, eight, nine, ten, or more than ten times. Preferably, the neutralised LM amidated pectin is washed with the alcohol three times.
[000144] Preferably, the pH adjusted LM amidated pectin is washed with alcohol at from 50 to 70 weight %, or, from 55 to 65 weight %, or, at 60 weight % of the total weight of the alcohol.
[000145] The second-washed LM amidated pectin can undergo a drying step to form a dried LM amidated pectin.
[000146] Preferably, the drying step is carried out by press-drying.
[000147] Preferably, the second-washed LM amidated pectin can be dried until the dried LM amidated pectin has a moisture content of from 1 to 30 weight %, or from 2 to 20 weight &, or from 7.5 to 15.0 weight 5, or from 9 to 11 weight %, or. 10 weight % of the total weight of the dried LM amidated pectin.
[000148] The dried LM amidated pectin is a LM amidated pectin ready for use in a composition according to the present invention. The dried LM amidated pectin can be blended with sugar to form a standardised LM amidated pectin.
[000149] For the product of the second step to be the pectin of the present invention, some key parameters of the above process need to be controlled in the amidation reaction. The parameters include the of alcohol and ammonia weight % in the suspension, the residence time of the HM pectin in the suspension and the temperature of the suspension. By controlling these parameters, the desired degree of esterification and degree of amidation can be obtained.
[000150] Preferably, the weight % of the ammonia in the suspension is at from 2.8 to 3.5 weight % of the total weight of the suspension. Preferably, the w eight % of the weight % of the alcohol in the suspension is 60 to 70 weight % of the total weight of the suspension Preferably, the residence time is maintained for from 5 to 8 hours. Preferably, the reaction temperature is maintained at from 10 to 14°C. Preferably, weight % of the ammonia in the suspension is at from 2.8 to 3.5 weight % of the total weight of the suspension, the weight % of the alcohol in the suspension is 60 to 70 weight % of the total weight of the suspension, the residence time is maintained for from 5 to 8 hours and the reaction temperature is maintained at from 10 to 14°C.
Method of making the composition comprising a pectin
[000151 ] Another aspect of the present invention relates to a method of making a composition, wherein the composition comprises a pectin and water. The method of making the composition comprises the following steps:
(a) providing a pectin;
(b) combining the pectin with water to form a composition.
[000152] The composition may comprise the pectin at a concentration of from 0.001 to 10 weight % relative to the total amount of pectin and water, preferably from 0.01 to 7.5 weight % relative to the total amount of pectin and water, more preferably from 0.1 to 5 weight % relative to the total amount of pectin and water, even more preferably from 0.2 to 3 weight % relative to the total amount of pectin and water, even more preferably from 0.3 to 2.5 weight % relative to the total amount of pectin and water, most preferably from 0.4 to 2 weight % relative to the total amount of pectin and water.
[000153] The composition may additionally comprise a gel-promoting medium at from 0.001 to 10 mM, preferably from 0.005 to mM, most preferably from 0.01 to 8 mM. Preferably, the gel-promoting medium is calcium.
[000154] Preferably, the composition comprises pectin at a concentration of from 0.4 to 2 weight % of the total weight of the composition and calcium (as a gel-promoting medium) at from 0.01 to 8 mM.
[000155] The composition may additionally comprise sugar. The composition may comprise the sugar at from 20 to 60 weight %, or, from 30 to 50 weight %, or, from 35 to 45 weight %, or at 40 weight % of the total weight of the composition. Preferably, the sugar is, but not limited to. sucrose, dextrose, lactose, maltose, glucose and/or galactose.
Method of making a composition as a pectin gel
[000156] Another aspect of the present invention relates to a method of making a pectin gel, wherein the pectin gel comprises a composition as set out under the heading “Composition’; i.e., wherein the pectin gel comprises pectin and water. The method of making the pectin gel comprises the following steps:
(a) combining pectin, a gel-promoting medium and water to form a solution;
(b) heating the solution until the pectin and gel-promoting medium dissolve;
(c) cooling the pectin solution to form a gel.
[000157] Preferably, the pectin is at a concentration of from 0.001 to 10 weight % of the total weight of the pectin gel. preferably from 0.01 to 7.5 weight % of the total weight of the pectin gel, more preferably from 0.1 to 5 weight % of the total weight of the pectin gel, even more preferably from 0.2 to 3 weight % of the total weight of the pectin gel, even more preferably from 0.3 to 2.5 weight % of the total weight of the pectin gel, most preferably from 0.4 to 2 weight % of the total weight of the pectin gel. Preferably, the gel-promoting medium is at a concentration of from 0.001 to 10 mM, preferably from 0.005 to 9 mM, most preferably from 0.01 to 8 mM. Preferably, the gel-promoting medium is calcium. Preferably, the pectin is at a concentration of from 0.4 to 2 weight % of the total weight of the pectin gel and the gelmedium cation is at a concentration of from 0.01 to 8 mM.
[000158] Preferably, the solution is heated to from 70 to 110 °C, preferably from 75 to 105 °C, most preferably from 80 to 95 °C. Preferably, the solution is heated from a duration of from 1 to 60 minutes, preferably from 5 to 45 minutes, most preferably from 10 to 30 minutes. Preferably, the solution is heated to from 80 to 95 °C for a duration of 10 to 30 minutes.
[000159] Preferably, the solution is cooled to a temperature of from 1 to 30 °C, preferably from 5 to 25 °C. most preferably from 10 to 20 °C.
The composition in a food or beverage product [000160] Another aspect of the present invention relates to the composition in a food or beverage product, wherein the composition is as set out under the heading '‘Composition”.
[000161] The composition may be incorporated into a daily' product, which includes, but is not limited to, milk, condensed milk, dried milk, milk-drinks, cream, butter, yoghurt, cheese, custard, cottage cheese, cream cheese, curd, frozen dairy products such as frozen custard, frozen yogurt and ice-cream, gelato, powdered milk, evaporated milk, sour cream, soured milk, whey, whey protein or whipped cream.
[000162] The composition may be incorporated into a sweet product, which includes, but is not limited to, a confectionary product, reduced sugar jams, fruit preparations, jellies, glazes and spray glazes.
[000163] Preferably, the composition is incorporated into a meat product, a poultry’ product, a fish product, dairy products such as milk, ice cream, yoghurt, cheese, pudding, and flavoured dairy drinks, baked foods such as bread, cake, cookies, crackers, biscuits, pies, donuts, pretzels, and potato chips, non-dairy spreads, mayonnaise, soups, sauces, dips, dressings, frozen confections, fruit preparations, jams and jellies, beverages, water gels, confectionery jelly or low-fat spreads.
The composition in a non-food or non-beverage product
[000164] Another aspect of the present invention relates to the composition in a non-food or a non-beverage product, wherein the composition is as set out under the heading “Composition”.
[000165] The composition may be incorporated into other products related to nutraceuticals, biological activities, cosmetics and pharmaceutics.
Method of producing the composition in a food or beverage product
[000166] Another aspect of the present invention relates to a method of making a food or beverage product comprising the composition, wherein the composition is as set out under the heading “Composition’". The method of making the food or beverage product comprises the steps:
(a) providing the composition; and
(b) combining the composition with at least one food or beverage product.
Method of producing the composition in a non-food or non-beverage product
[000167] Another aspect of the present invention relates to a method of making a non-food or non-beverage product comprising the composition, wherein the composition is as set out under the heading “Composition”. The method of making the non-food or non-beverage product comprises the steps:
(a) providing the composition; and
(b) combining the composition with at least one non-food or non-beverage product.
EXAMPLES
[000168] The following are non-limiting examples that discuss, with reference to tables and figures, the advantages of the present invention. The examples set forth herein are merely examples among other possible examples.
The materials used in the examples
[000169] Novel pectins were made according to the method set out in Example 1.
[000170] The novel pectins were compared to commercially available pectins, provided by Cargill, Incorporated.
[000171] The pectin samples are listed in Table 1. Table 1: Pectin samples used in the evaluation of the present invention.
[000172] The composition of the commercially available pectins is set out in Table 2.
Table 2: The composition of the commercially available pectins.
*wherein GalA is the galacturonic acid (GalA) content of each pectin.
Example 1: Extraction of an LM amidated pectin
Step 1: Extraction of HM pectin
[000173] First, citrus peel or apple pomace was mixed in acidic, hot water to extract the HM pectin from the citrus peel or apple pomace as a HM pectin in aqueous form. The temperature of the acidic, hot water was from 68 to 72°C, the pH was from pH 1.50 to 1.70 and the residence time was from 8 to 12 hours.
[000174] The HM pectin in aqueous form was clarified by using centrifugation and filtered to form a clarified HM pectin in aqueous form.
[000175] The clarified HM pectin in aqueous form was then concentrated to form a concentrated HM pectin in aqueous form.
[000176] Isopropyl alcohol was added to the concentrated HM pectin in aqueous form to cause the HM extract to precipitate out as a precipitate containing the HM pectin. The precipitate containing the HM pectin was present in an alcohol (isopropyl alcohol) / water mix.
[000177] The precipitate containing the HM pectin was separated from the alcohol/water mix by mechanical separation.
[000178] The precipitate containing the HM pectin obtained from the separation was then washed three times with isopropyl alcohol at 60 weight % of the total weight of the alcohol to form a washed HM pectin.
[000179] The washed HM pectin then underw ent a drying step to form a dry HM pectin. The drying step dried the washed precipitate containing the HM pectin until the washed precipitate containing the HM pectin had a moisture content of 10 weight % of the total weight of the dry HM pectin.
Step 2: Amidation of dry HM pectin
[000180] The dry HM pectin was placed in a suspension which comprised alcohol (isopropyl alcohol) and ammonia. The alcohol was present at from 60 to 70 weight % of the total weight of the suspension and the ammonia was present at 2.8 to 3.5 weight % of the total weight of the suspension. The suspension was maintained at a temperature of from 10 to 14 °C. The dry HM pectin was in the suspension for from 5 to 8 hours. Once 5 to 8 hours had passed, the dry HM pectin had undergone amidation to form LM amidated pectin.
[000181] To stop further reaction occurring in the suspension, the LM amidated pectin was fdtered out from the alcohol and ammonia. The alcohol and ammonia passed to a recover}' step. The LM amidated pectin was washed with isopropyl alcohol at 60 weight % of the total weight of the alcohol to form a washed LM amidated pectin.
[000182] The pH of the washed LM amidated pectin was adjusted to form a pH adjusted LM amidated pectin. The pH of the washed LM amidated pectin w as adj usted until the pH was between 4.0 to 4.5. The pH was adjusted with nitric acid.
[000183] The pH adjusted LM amidated pectin was washed with isopropyl alcohol three times to form a second-washed LM amidated pectin.
[000184] The second-washed LM amidated pectin underwent a drying step to form a dried LM amidated pectin. The drying step dried the second-washed LM amidated pectin until the second-washed LM amidated pectin had a moisture content of 10 weight % of the total w eight of the dried LM amidated pectin.
[000185 ] Example 2: Structural characterisation of a LM amidated pectin
[000186] In this non-limiting example of the present invention, the degree of esterification (DE), degree of amidation (DA) and galacturonic acid content (GalA) of a pectin were determined using a titration method (as set out in National Research Council, 1981, Yu, et al, 2021, the disclosure of which is hereby incorporated by reference in its entirety). The method of measuring the degree of esterification (DE), degree of amidation (DA) and galacturonic acid content (GalA) includes washing the pectin samples with acidified aqueous isopropanol to remove any cations, salts and standardising sugars. The purified pectin is then titrated with 0.1 M sodium hydroxide. The ester groups are saponified with an excess of 0.5 M sodium hydroxide, which is then neutralised with an exactly equivalent amount of 0.5 M hydrochloric acid, enabling the liberated acid groups to be titrated with 0.1 M sodium hydroxide. The solution may then be distilled with strong alkali to liberate ammonia from the amide groups of amidated pectins. By the back titration procedure, the ammonia is estimated in terms of the same 0.1 M sodium hydroxide. After the titrations, the proportions of the degree of amidation, the degree of esterification and galacturonic acid content were calculated following the procedure described in National Research Council, 1981, Yu, et al, 2021, the disclosure of which is hereby incorporated by reference in its entirety.
[000187] The degree of amidation, the degree of esterification and galacturonic acid content of the LM amidated pectin is shown in Table 3.
Table 3: The chemical composition of the pectin.
Example 3: Measuring the intrinsic viscosity of the LM amidated pectin
[000188] In this non-limiting example of the present invention, the intrinsic viscosity of the pectins was determined by size-exclusion chromatography-Multi-Angle Laser Light Scattering (SEC-MALLS) as descnbed in Hellin, P„ Ralet, M. C , Bonnin, E„ & Thibault, J. F. (2005).
Homogalacturonans from lime pectins exhibit homogeneous charge density and molar mass distributions. Carbohydrate Polymers, 60(3), 307-317, and in particular on page 309 (where the method of determining the intrinsic viscosity of the pectins in disclosed), the disclosure of which is hereby incorporated by reference in its entirety.
[000189] Pectin solutions at 5 mg/mL in water were prepared in 50 mM sodium nitrate containing 0.02 weight % sodium azide as a preservative. The intrinsic viscosity was calculated using Astra software (Wyatt, Santa Barbara, CA, the disclosure of which is hereby incorporated by reference in its entirety) and the TriSec software (Version 3.0, Voscotek. Houston. TX, the disclosure of which is hereby incorporated by reference in its entirety). All analysis was performed in triplicate, and the mean value taken.
[000190] The mean value for the intrinsic viscosity of the pectins is shown in Table 4.
Table 4: The intrinsic viscosity of the pectins.
Example 4: Makins a composition comprising a LM amidated pectin and water
[000191] In this non-limiting example, separate compositions comprising each pectin as shown in Table 1 were made. The compositions comprised pectin and water: each composition comprised one of pectins 1-5. The compositions were prepared so that the resultant pectin concentrations were at from 0.4 to 2.0 weight % with sucrose (at 40 weight %) of the total weight of the composition.
[000192] To prepare each composition, pre-solutions of pectin were first prepared by dissolving each pectin separately in distilled water under mechanical stirring for 10 minutes at 90°C. [000193] After dissolution of the pectin in the distilled water, from 190 to 320 g of a hot buffer solution and a gel-promoting medium were added to the distilled water and pectin solution.
[000194] The buffer comprised sodium citrate at a sufficient concentration so that the pH of the buffer was at 3.4. The sodium citrate was dissolved in distilled water. Prior to adding the buffer to the distilled water and pectin solution, the buffer was heated to the same temperature as the distilled water and pectin solution (90°C). The buffer solution also contained CaCh (at 8.4 mM) and sucrose.
[000195] The gel-promoting medium was added to the solution comprising the distilled water and pectin at a concentration of 8.4 mM in water. The composition of the gel-promoting medium is set out in Table 5.
Table 5: Gel-promoting medium.
*fbr 5 litres of pH 3.4 buffer stock solution.
[000196] Advantageously, the ionic strength of the gel -promoting medium plays an important role on the temperature of gelation critical gelling concentration. The higher the ionic strength of the gel-promoting medium, the higher the gelation of temperature and the lower the critical gelling concentration.
[000197] The resulting composition, having a final calcium chloride (CaCh) concentration of 3 mM, was kept under stirring (at 90°C) for 5 minutes. The final pH of each composition prepared was 3.4.
[000198] Table 6 shows which composition contains which pectin.
Table 6: The pectin used to make each composition.
Example 5: Measuring the temperature of gelation (T g)
[000199] In this non-limiting example, the temperature of gelation (Tg) was measured for each composition. The temperature of gelation (Tg) was measured over a pectin concentration ranging from 0.8 weight % to 1.4 weight % (of the total weight of the composition) for each composition.
[000200] The compositions analysed are the compositions produced in Example 4.
[000201] To measure the temperature of gelation (Tg) of each composition, dynamic oscillatory (or small deformation) measurements were carried out using either an ARES-G2 strain-controlled rheometer (TA Instruments) or a MCR 92 stress-controlled rheometer (Anton Paar Physica) on each composition separately. Both rheometers are equipped with a Couette device.
[000202] For the measurements, each composition (as described above in Example 4) was covered by a thin layer of paraffin oil to avoid evaporation during measurements.
[000203] Before a measurement was taken, each composition was poured (separately) into the Couette device (pre-heated at 80°C) and was first pre-sheared (at 10 s’1 for 2 min) to clean the loading history of the composition. The composition was then exposed to a temperature sweep test (2°C/min) from 80°C down to 10°C. The viscoelastic experiments performed using the ARES-G2 strain-controlled rheometer and the MCR 92 stress-controlled rheometer were carried out at 0.4% and 10% of strain, respectively, and at a frequency of 0.8 Hz. Both strain amplitudes were verified to be in the LVE domain. [000204] In all these small deformation experiments, each measurement was performed in triplicate, from new composition preparations (of the same composition). The mean value was taken from the triplicate measurements.
[000205] At the end of the measurements, the gelation temperature (Tg) representing the cross-over point between storage modulus (G’) and loss modulus (G ") was collected from the gelation kinetic data obtained after the temperature sweep test (described above). The storage modulus G’ and loss modulus (G: ’) values were collected from the mechanical spectra using an automatic data exporting program from the Rheocompass software (from Anton Paar company). The cross-over point between the storage modulus (G’) and loss modulus (G’‘) was determined, as illustrated in FIG. 2. FIG. 2 shows data points for Composition 1 at 1.4 % pectin concentration in water. Then, the mean value of Tg and corresponding standard deviation of the obtained data in triplicate was calculated.
[000206] The measurements were then repeated for each composition (separately).
[000207] The mean value for the temperature of gelation (Tg) measurements are shown in
Table 7.
Table 7: The mean value for the temperature of gelation (Tg) for each composition.
Example 6: Measuring the critical gelling concentration (Co)
[000208] In this non-limiting example, the critical gelling concentration was measured for each composition. [000209] The compositions analysed are the compositions produced in Example 4.
[000210] To measure the critical gelling concentration, dynamic oscillatory (or small deformation) measurements were carried out using either an ARES-G2 strain-controlled rheometer (TA Instruments) or a MCR 92 stress-controlled rheometer (Anton Paar Physica). Both rheometers are equipped with a Couette device.
[000211] For these measurements, each composition prepared as described above was covered by a thin layer of paraffin oil to avoid evaporation during measurements.
[000212] Before measurements, each composition was poured (separately) into the Couette device (pre-heated at 80°C) and was first pre-sheared (at 10 s'1 for 2 min) to clean the loading history of the device. Each composition was then exposed to a temperature sweep test (2°C/min) from 80°C down to 10°C. followed by a time sweep experiment for 30 minutes at a frequency of 0.8 Hz to ensure that the resulting gel reaches an equilibrium state due to reorganization (structural rearrangements). To ensure that viscoelastic measurements were carried out in the LVE domain, strain sweep experiments were conducted from 0.01% to 40% at 0.8 Hz. The viscoelastic experiments performed using the ARES-G2 strain-controlled rheometer and the MCR 92 stress- controlled rheometer, were carried out at 0.4% and 10% of strain, respectively. Both strain amplitudes were verified to be in the LVE domain.
[000213] In all these small deformation experiments, each measurement was performed in triplicate, from new composition preparations (of the same composition). The mean value was taken.
[000214] Then, the following steps were carried out for the determination of Co:
(i) the storage modulus (G’) values and loss modulus (G'’) values were collected from the mechanical spectra using an automatic data exporting program from the Rheocompass software (from Anton Paar company) and was plotted as a function of the pectin concentration, C (%), in logarithmic scales, an example of such a plot is illustrated in FIG. 3, which shows the experimental data and calculated data for the storage modulus (G’) as a function of pectin concentration for Composition 1 (the calculated data was obtained by using the equation G’ = 1700*(C- Co)2 19 with Co = 0.05%, as shown in FIG. 3; the second equation (G = 1733.2*C2 19, R2 = 0.9974) shown on FIG. 3 refers to the fitting model of the experimental data, where the exponential value reflects the structural level of the gel and R2 is a statistical measure of fit that indicates how much variation of a dependent variable is explained by the independent values in a regression model: when R2 is close to one (as with this case), the fitting model is robust);
(ii) the data was fitted using a power-law relationship to obtain the equation G’= AC". where G’ is the storage modulus, k represents the scaling factor, C (%) the pectin concentration and n an exponent value (the equations for the calculated and experimental data are shown above in step (i)); and
(iii) following the approach described in literature (e.g. de Gennes, P.-G. (1979). Scaling Concepts in Polymer Physics. Cornell University Press: Ithaca and London, New York.; Jones, J. L., & Marques, C. M. (1990). Rigid polymer network models. Journal de Physique. 51. 1113- 1127. ; Ross-Murphy, S. B. (1987) and Physical gelation of biopolymers. Food Hydrocolloids, 7, 485-495., the disclosures of which are hereby incorporated by reference in its entirety), the equation G’= AC” was mathematically transformed into the form G’= k’(C- Co)n using linear regression. In this second equation, k ' represents the scaling factor and Co the concentration below which no gel-like behaviour can be achieved.
[000215] The linear regression was performed for all investigated products following the condition G’= ACn = k (C- Co)n. with both exponents (n) values being identical and C > Co.
[000216] The validation of critical gelling concentration (Co) determined using the above fitting model w as then verified by evaluating the rheological behaviour of Compositions 1, 2, 3, 4 and 5 in the same conditions.
[000217] The measurements were then repeated for each composition (separately). Each measurement w as performed in triplicate for each composition preparations, and the mean value taken.
[000218] The mean value of the critical gelling concentration (Co) measurements are shown in Table 8.
Table 8: The mean value of the critical gelling concentration (Co) for each composition.
[000219] Advantageously, a low critical gelling concentration (Co) results in a highly functional product. The lower the critical gelling concentration (Co) of the composition, the less of the composition that is required in a food and/or beverage product to obtain a gel. The compositions of the present invention have a low critical gelling concentration (Co) and therefore less of the composition will be required in a food and/or beverage product to obtain a gel. This advantageously results in a food and/or beverage product which is cheaper to manufacture, because less of the composition is required in the food and/or beverage product.
[000220] Further advantageously, the lower the ratio of degree of esterification (DE) to degree of amidation (DA), the lower the critical gelling concentration (Co).
[000221] Further advantageously, the above-mentioned advantage for end-used product formulation can help identify novel routes of rational product formulation (thus allowing the cost-in-use to be reduced) and continuously optimises pectin processing conditions.

Claims

1. A composition having a temperature of gelation (Tg), comprising: a pectin; and, water; wherein when the concentration of the pectin in the water is increased from 0.8 weight % to 1.4 weight % relative to the total weight of the composition, the temperature of gelation (Tg) varies by from 0.5 to 2.5 °C.
2. The composition of claim 1 wherein when the pectin concentration in the water is increased from 0.8 weight % to 1.4 weight % relative to the total weight of the composition, the temperature of gelation (Tg) varies by from 0.50 to 2.0 °C, or, from 0.75 to 1.5 °C, or, from 1.0 to 1.3 °C, or, from 1.03 to 1.27 °C; and/or wherein the pectin has a degree of esterification (DE) of from 15 to 45 %, or from, 18 to 40 %, or, from 20 to 35 %, or, from 23 to 31 %, or, from 23.3 to 31.0 %; and/or, wherein the pectin has a degree of amidation (DA) of from 5 to 30 %, or, from 12 to 25 %. or, from 15 to 23 %, or, from 16.0 to 22.1 %; and/or, wherein the pectin has a ratio of a degree of esterification (DE) to a degree of amidation (DA) of from 0.75 to 3.0, or, from 0.85 to 2.5, or, from 0.95 to 2.0, or, from 1.05 to 1.94.
3. The composition of claim 1 or claim 2, wherein when the pectin concentration in the water is increased from 0.8 weight % to 1.4 weight % relative to the total weight of the composition, the temperature of gelation varies by 1.27°C; optionally, wherein the pectin has a ratio of a degree of esterification (DE) to a degree of amidation (DA) of 1.94.
4. The composition of claim 1 or claim 2, wherein when the pectin concentration in the water is increased from 0.8 weight % to 1.4 weight % relative to the total weight of the composition, the temperature of gelation (Tg) varies by 1.03°C; optionally, wherein the pectin has a ratio of a degree of esterification (DE) to a degree of amidation (DA) of 1.05.
5. The composition of any one of claims 1 to 4, wherein the pectin is low methoxyl (LM) amidated pectin; optionally, wherein the low methoxyl (LM) amidated pectin has a degree of methylation of below 50 %; and/or, wherein the degree of esterification (DE) is measured by titration; and/or, wherein the degree of amidation (DA) is measured by titration; and/or, wherein the temperature of gelation (Tg) is measured by dynamic oscillatory rheological measurements.
6. A pectin having: a degree of esterification (DE) of from 15 to 45 %, or from, 18 to 40 %, or, from 20 to 35 %, or, from 23 to 31 %. or 23.3 to 31 %. a degree of amidation (DA) of from 5 to 30 %, or. from 12 to 25 %. or. from 15 to 23 %, or, from 16 to 22.1 ; and, a ratio of a degree of esterification (DE) to a degree of amidation (DA) of from 0.75 to 3.0, or, from 0.85 to 2.5, or, from 0.95 to 2.0, or, from 1.05 to 1.94.
7. A composition having a critical gelling concentration (Co) comprising: a pectin; and, water; and wherein the critical gelling concentration (Co) is from 0.01 to 0.2 weight %.
8. The composition of claim 7, wherein the critical gelling concentration (Co) is from 0.02 to 0.17 weight %, or, from 0.025 to 0.15 weight %, or, from 0.04 to 0.13 weight %, or, from 0.05 to 0.12 weight %; and/or, wherein the pectin has a ratio of a degree of esterification (DE) to a degree of amidation (DA) of from 0.75 to 3.0, or, from 0.85 to 2.5, or, from 0.95 to 2.0, or, from 1.05 to 1.94; and/or, wherein: the critical gelling concentration (Co) is 0.12 weight %; optionally. wherein the pectin has a ratio of a degree of esterification (DE) to a degree of amidation (DA) of 1.94; or, wherein: the critical gelling concentration (Co) is 0.05 weight %; optionally, wherein the pectin has a ratio of a degree of esterification (DE) to a degree of amidation (DA) of 1.05.
9. The composition of claim 7 or claim 8, wherein the pectin is a low methoxyl (LM) amidated pectin; optionally, wherein the low methoxyl (LM) amidated pectin has a degree of methylation of below 50 %; and/or, wherein the degree of esterification (DE) is measured by titration; and/or, wherein the degree of amidation (DA) is measured by titration; and/or, wherein the critical gelling concentration (Co) is measured by dynamic oscillatory rheological measurements.
10. A composition having a temperature of gelation (Tg) and a critical gelling concentration (Co) comprising: a pectin; and, water; wherein when the pectin concentration in the water increases from 0.8 weight % to
1.4 weight % relative to the total weight of the composition, the temperature of gelation (Tg) varies by from 0.5 to 2.5 °C; and wherein the critical gelling concentration (Co) is from 0.01 to 0.2 weight %.
11. The composition of claim 10 wherein when the pectin concentration in the water is increased from 0.8 weight % to 1.4 weight % relative to the total weight of the composition, the temperature of gelation (Tg) varies by from 0.50 to 2.0 °C, or, from 0.75 to 1.5 °C, or, from 1.0 to 1.3 °C. or, from 1.03 to 1.27 °C; and/or. wherein the critical gelling concentration (Co) is from 0.02 to 0.17 weight %, or, from 0.025 to 0.15 weight %, or. from 0.04 to 0.13 weight %, or, from 0.05 to 0. 12 weight %; and/or, wherein the pectin has a ratio of a degree of esterification (DE) to a degree of amidation (DA) of from 0.75 to 3.0, or. from 0.85 to 2.5. or, from 0.95 to 2.0, or, from 1.05 to 1.94; and/or. wherein the pectin is low methoxyl (LM) amidated pectin; optionally, wherein the low methoxyl (LM) amidated pectin has a degree of methylation of below 50 %; and/or, wherein the degree of esterification (DE) is measured by titration; and/or, wherein the degree of amidation (DA) is measured by titration; and/or, wherein the temperature of gelation (Tg) and/or the critical gelling concentration (Co) is measured by dynamic oscillatory rheological measurements.
12. The composition of any one of claims 1 to 1 1, wherein the pectin is sourced from apple pomace and/or citrus peel; and/or, wherein the composition further comprises sugar, optionally, wherein the sugar is any one of sucrose, dextrose, lactose, maltose, glucose and/or galactose; optionally, wherein the sugar is present at from 20 to 60 weight %, or, from 30 to 50 weight %, or, from 35 to 45 weight %, or at 40 weight % relative to the total weight of the composition.
13. A method of making a composition according to any one of claims 1 to 12, the method comprising the following steps: obtaining a high methoxyl (HM) pectin in aqueous form from a natural source; drying the high methoxyl (HM) pectin in aqueous form to form a dry high methoxyl (HM) pectin, wherein the dry high methoxyl (HM) pectin has a moisture content of 10 weight % of the total weight of the dry high methoxyl (HM) pectin; placing the dry high methoxyl (HM) pectin in a suspension comprising alcohol and ammonia to form an amidated low methoxyl (LM) pectin; drying the amidated low methoxyl (LM) pectin to form a dried amidated low methoxyl (LM) pectin, wherein the dried amidated pectin has a moisture content of 10 w eight % of the total weight of the dried amidated low methoxyl (LM) pectin; adding water to the amidated low' methoxy l (LM) pectin to form a composition.
14. The method of claim 13, wherein the natural source is any one of apples, apple pomace, citrus peel, lemons, mandarin oranges, grapefruit, sweet orange, pomelo, clementines, limes, kumquat, bitter oranges, blood oranges, satsumas, yuzus, tangelos, or, any combinations thereof; and/or, wherein the natural source is apple pomace or citrus peel; and/or, further comprising any one or more of the following steps: clarifying the high methoxyl (HM) pectin in aqueous form; optionally wherein the high methoxyl (HM) pectin in aqueous form is clarified by centrifugation and/or filtration; concentrating the high methoxyl (HM) pectin in aqueous form; washing the high methoxyl (HM) pectin in aqueous form with alcohol; subjecting the high methoxyl (HM) pectin in aqueous form to a separation process; optionally, wherein the separation process is mechanical separation. filtering the ami dated low methoxyl (LM) pectin; washing the amidated low methoxyl (LM) pectin with alcohol; and/or adjusting the pH of the amidated low methoxyl (LM) pectin.
15. Use of the composition according to any one of claims 1 to 12 in a food and/or beverage product.
EP24721831.6A 2023-04-06 2024-04-01 A composition comprising a pectin and water Pending EP4688942A1 (en)

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US2480710A (en) 1945-11-07 1949-08-30 Fruit Growers Exchange Ca Acid amides of pectinic acid and process for their preparation
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ATE299152T1 (en) 1999-03-31 2005-07-15 Cp Kelco Aps PECTIN WITH REDUCED CALCIUM REACTIVITY
US6428837B1 (en) 2000-06-09 2002-08-06 Cp Kelco Aps Deesterified pectins, processes for producing such pectins, and stabilized acidic liquid systems comprising the same
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