WO1991015517A1 - Produit contenant de la pectine et procede de fabrication - Google Patents

Produit contenant de la pectine et procede de fabrication Download PDF

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Publication number
WO1991015517A1
WO1991015517A1 PCT/DK1991/000072 DK9100072W WO9115517A1 WO 1991015517 A1 WO1991015517 A1 WO 1991015517A1 DK 9100072 W DK9100072 W DK 9100072W WO 9115517 A1 WO9115517 A1 WO 9115517A1
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WIPO (PCT)
Prior art keywords
water
product
weight
acid
pectin
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PCT/DK1991/000072
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English (en)
Inventor
Hans Christian Buchholt
Hasse Vinter
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Grindsted Products A/S (Danisco A/S)
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Application filed by Grindsted Products A/S (Danisco A/S) filed Critical Grindsted Products A/S (Danisco A/S)
Publication of WO1991015517A1 publication Critical patent/WO1991015517A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
    • C08B37/0045—Homoglycans, 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
    • C08B37/0048—Processes of extraction from organic materials
    • A—HUMAN NECESSITIES
    • A21—BAKING; EDIBLE DOUGHS
    • A21D—TREATMENT, e.g. PRESERVATION, OF FLOUR OR DOUGH, e.g. BY ADDITION OF MATERIALS; BAKING; BAKERY PRODUCTS; PRESERVATION THEREOF
    • A21D15/00—Preserving finished, partly finished or par-baked bakery products; Improving
    • A21D15/02—Preserving finished, partly finished or par-baked bakery products; Improving by cooling, e.g. refrigeration, freezing
    • A—HUMAN NECESSITIES
    • A21—BAKING; EDIBLE DOUGHS
    • A21D—TREATMENT, e.g. PRESERVATION, OF FLOUR OR DOUGH, e.g. BY ADDITION OF MATERIALS; BAKING; BAKERY PRODUCTS; PRESERVATION THEREOF
    • A21D2/00—Treatment of flour or dough by adding materials thereto before or during baking
    • A21D2/08—Treatment of flour or dough by adding materials thereto before or during baking by adding organic substances
    • A21D2/14—Organic oxygen compounds
    • A21D2/18—Carbohydrates
    • A21D2/183—Natural gums
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L21/00—Marmalades, jams, jellies or the like; Products from apiculture; Preparation or treatment thereof
    • A23L21/10—Marmalades; Jams; Jellies; Other similar fruit or vegetable compositions; Simulated fruit products
    • A23L21/12—Marmalades; Jams; Jellies; Other similar fruit or vegetable compositions; Simulated fruit products derived from fruit or vegetable solids
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L21/00—Marmalades, jams, jellies or the like; Products from apiculture; Preparation or treatment thereof
    • A23L21/10—Marmalades; Jams; Jellies; Other similar fruit or vegetable compositions; Simulated fruit products
    • A23L21/18—Simulated fruit products
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/206—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
    • A23L29/231—Pectin; Derivatives thereof
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/20—Reducing nutritive value; Dietetic products with reduced nutritive value
    • A23L33/21—Addition of substantially indigestible substances, e.g. dietary fibres
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
    • A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
    • A61L15/22—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing macromolecular materials
    • A61L15/28—Polysaccharides or their derivatives

Definitions

  • the present invention provides a novel low-cost crude pectin-containing vegetable product prepared from agricul- tural waste products and a method for the production there ⁇ of.
  • the product comprises 5-45% pectic substances of which at least 10% are in a water-soluble form.
  • the pectic sub ⁇ stances of the product has a degree of esterification in the range of 45-90%.
  • the product is useful as thickening and gelling agents, as a water absorbing and/or water holding agent and as a dietary fibre additive especially for lowering the cholesterol levels in the blood.
  • the method of production which is provided comprises a treat ⁇ ment of the starting material with an acid, an acid-produc- ing microorganism or a suitable enzyme to obtain conversion of at least part of the water-insoluble pectic substances to water-soluble pectin, under conditions where water is added in an amount which will result in a water content not substantially higher than the original water content of the starting vegetable material in its fresh state.
  • pectic substances is used to cover a group of colloidal heteropolysaccharides found in plants and com ⁇ posed predominantly of polygalacturonic acids formed by the chainlike combination of anhydrogalacturonic acid residues. Some of the carboxyl groups of the polygalacturonic acids are esterified with methanol and some are usually neutral ⁇ ized by one or more alkaline substances. When occurring in plant tissues, pectic substances are in a water-insoluble form for which the general term protopectin is used. When subjected to restricted hydrolysis, protopectin yields pectinic acids which are polygalacturonic acids of col ⁇ loidal nature in which some of the carboxyl groups are esterified with methyl groups.
  • pectin designates pectinic acids which contain at least about 3% methyl ester groups, expressed as methoxyl, and which are capable of forming gels with in the presence of sugar and acid under suitable conditions.
  • pectic substances contain L-rhamnose residues which are bound to the main chains of polygalacturonic acids. These L-rhamnose residues act as sites for a more random branching comprising other sugars such as D-glucose, D-galactose, L-arabinose, D- xylose, D-mannose, and L-fucose whose occurrence vary from one pectin source to another. Branching is also known to occur at sites of some of the galacturonic acid residues. As a result of this branching, pectin can build up a hydro- philic three-dimensional network with a considerable water holding capacity. In general, pectin comprises 60-70% galacturonic acid.
  • Pectin occurs in all higher land plants, especially vas ⁇ cular plants in all parts of the plants e.g. in roots, stems, leaves, and particularly in fruits such as apples, lemons and lime where it is located in the primary cell walls and in the middle lamellas in the form of water- insoluble protopectin, together with cellulose and pen- tosans.
  • the molecular weight of water-soluble pectin resul- ting from hydrolysis of protopectin varies considerably but is typically less than 200000.
  • pectic substances as they occur in plants is not completely understood. There is, however, a very complex molecular arrangement between protopectin and the other cell wall components involving covalent and hydrogen bonds. Furthermore, metal ions such as Ca ++ and Mg ++ are also involved by complex binding to the pectic substance.
  • the main sources of commercial pectin products are citrus peel and apple pomace in which protopectin represents 10- 40% of the dry weight. Pectin is mostly obtained from the plant material by treating the material with an acid or a base under suitable conditions, whereby the protopectin is split, followed by extraction of the water-soluble pectin.
  • pectin acid or base treated plant starting material is subjected to a subsequent ex ⁇ traction with dilute acid, which step is followed by sepa- rating the depectinated plant material by e.g. filtration or centrifugation to obtain a viscous extract containing up till 1% soluble pectin. This extract may be purified and processed further. Finally, the pectin is precipitated, separated and dried to obtain the commercial pectin pro- d ct.
  • Pectin is commonly known for its gelling properties, the degree of which depends on the proportion of galacturonic acid residues which are in methyl ester form.
  • Commercial pectin products used as gelling agents fall into two groups: (1) High-methoxylated pectins with a degree of esterification higher than 45% and (2) low- ethoxylated pectins having a degree of esterification less than 45%.
  • Pectin is of significant importance in the food industry as a gelling and stabilizing agent in the manufacturing of food products such as jams, jellies, preserves, milk pro ⁇ ducts, cheese products, snacks and ice cream.
  • the gelling characteristics of pectin is utilized in other technical fields e.g. in the manufacturing of pet food, cosmetics, pharmaceuticals, paper, textiles and paints, and in the drilling industry.
  • pectic substances are classified as dietary fibres which also includes other complex polysaccharides of natural origin, e.g. alginates, carrageenan and agar from marine plants, gums and mucilages such as guar, ps Ilium seed gum and locust bean gum.
  • Seve ⁇ ral disorders, especially cardiovascular and gastrointes- tinal disorders prevailing in the human population in industrialized countries have been associated with shor ⁇ tages of dietary fibres in the daily diet.
  • dietary fibres have beneficial physiological effects such as a depression of blood serum cholesterol, improved blood glucose management in diabetic patients, lowering of blood pressure in hyper ⁇ tension, lowering of the risk of developing colon cancer, and aiding in control of body weight in overweight persons. Since dietary fibres comprise a rather diversified group of compounds it is not surprising that it has been found that the physiological effects thereof to some degree depend on the type of fibres and physical and chemical characteris ⁇ tics of the particular type of fibres.
  • pectin Amongst the beneficial physiological effects which have been associated with pectin, the ability hereof to reduce serum cholesterol levels (the hypocholesterolemic effect) in humans and in animals has during recent years attracted particular attention. Reported results from laboratory studies and human clinical trials are supportive evidence of this physiological effect. Based on results of feeding trials with rats it has also been demonstrated that highly esterified pectins are more effective in reducing choles ⁇ terol levels than low-esterified pectins.
  • pectin Major sources of raw materials for the production of pec- tin-containing products are vegetable waste products from juice processors, sugar beet refineries and other plant material processing industries.
  • pectin may be obtained in a substantially pure form by precipitating acid or alkaline extracts of vegetable materials, separating the precipitate which is optionally purified and subsequently dried.
  • a process for obtaining pectin products in substantially pure form involves considerable costs which seriously re ⁇ stricts the areas of application for such products.
  • GB 1.508.993 deals with a food product comprising a solid foodstuff and an aqueous phase which is thickened or gelled by a pectic substance with a degree of esterification less than 20% which substance is prepared by subjecting a natural pectin source, e.g. citrus peel to alkaline deesterification at a pH between 7 and 8 by treat ⁇ ment with an alkaline compound such as sodium carbonate.
  • a natural pectin source e.g. citrus peel to alkaline deesterification at a pH between 7 and 8 by treat ⁇ ment with an alkaline compound such as sodium carbonate.
  • a citrus fibre additive for grain flour is described in
  • US 4.225.628 which discloses a product obtained from citrus waste by neutralizing the natural acid content thereof by adding calcium hydroxide or oxide to obtain a pH of 5.5 to 7.0 and then pressing out water and soluble components.
  • the pressed material may be dried and used as is or it may be blended with a high protein flour prior to drying.
  • Another pectin-containing food additive which is useful as a tex ⁇ ture improving agent for various food products is disclosed in JP 56015654. This additive is prepared from the skin of citrus fruit which after extraction with an organic solvent to remove oily substances is reacted with alkaline calcium and/or magnesium compounds thereby partly converting the pectic substances to calcium and/or magnesium salts.
  • GB 2.145.103 discloses a highly water-absorbing pectin- containing product comprising from 15% to 60% pectin having a degree of esterification ranging from 1% to 45% and less than 50% of the pectin being in the form of a divalent metal salt.
  • Suitable raw materials are citrus pulp and sugar beet pulp.
  • the product is prepared by comminuting the vegetable material, deesterif ing the pectin contained therein to a degree of esterification of less than 45%, followed by a dewatering step, washing with water and finally drying the resulting material to obtain the pro ⁇ duct.
  • the step of deesterification may be carried out at acid or alkaline pH, but it is preferred to use an alkaline treatment since acid deesterification is too slow and re ⁇ sults in an undesirable extraction of divalent cations and degradation of hemicellulose.
  • the preferred alkaline de ⁇ esterification is carried out within a pH range of 9-12 at a temperature of 25°C or lower. It is stated that a degree of esterification of less than 45% is important to obtain satisfactory wicking properties of the absorbent material which properties are considered to be determinative for the water holding capacity.
  • US 4.497.838 discloses a product obtained by extraction of citrus peel with a non-aqueous water miscible solvent whereby sugars, essential oils and bioflavenoids are remo- ved from the peel. After drying and comminuting the sol ⁇ vent-extracted peel, a product is obtained which is rich in cellulose and pectic substances and having a high water holding capacity. The product is useful as a thickening, emulsifying or stabilizing agent and as a hypocholestero- lemic agent.
  • JP 63216822 discloses a cholesterol-lowering fibre composition prepared from sugar beets by removing soluble components by extraction with warm water.
  • JP 57054573 describes a dietary fibre product prepared by treating pressed sugar beet pulp with a weak hypochlorous acid solution at pH 6.5 to 7.5 followed by washing and drying.
  • Other dietary fibre products have been made by treating vegetable materials rich in fibres with solutions of bleaching agents such as hydrogen peroxide.
  • bleaching agents such as hydrogen peroxide.
  • the degree of esterification of water-soluble pectic sub- stances determines the physical and physiological charac ⁇ teristics of these useful compounds.
  • the majority of the commercial, substantially purified pectin products which are predominantly applied as gelling agents in the food industry have a degree of esterification of 45% or more.
  • the extraction of pectin is usually carried out under acidic conditions, since alkaline treatment enhances deesterification.
  • the present invention relates to a crude pectin product containing plant tissue material with microscopically recognizable plant tissue structures having a dry matter content of at least 85% wherein the dry matter comprises 5- 45% by weight of pectic substances having a degree of esterification of more than 45% of which pectic substances more than 10% is in a water-soluble form.
  • the dry matter further comprises 5-15% by weight of ashes comprising a proportion of alkaline and/or alkaline earth metals in the range of 30-50% by weight, and 40-90% by weight of non- pectic plant cell material comprising cellulose, hemicel- lulose, organic acids and water-soluble carbohydrates.
  • the product is further characterized in that the pH of a 1% aqueous suspension thereof is in the range of 3-5, the reduced viscosity of its water-soluble pectic substances is in the range of 0.050 to 0.500 L/g, and in that the water holding capacity is at least 4 g water/g, and in that it has a reducing effect on the levels of cholesterol in blood serum and liver of animals when fed thereto.
  • a product which is in the form of a substantially free- flowing powder consisting essentially of particles of a size of at the most 1.0 mm.
  • the present invention relates to a method for producing a product as defined above, which method comprises subjecting plant tissue material contain- ing pectic substances and having microscopically recog ⁇ nizable plant tissue structures to conditions which will convert at least part of the water-insoluble pectic sub ⁇ stances to water-soluble pectic substances in which sub ⁇ stances the degree of esterification initially present in the water-insoluble pectic substances is substantially preserved, followed by drying the resulting material to obtain the product with a water content of 15% by weight or less and optionally comminuting the dried material, sub ⁇ stantially without at any stage adding water in an amount which may result in a water content higher than the origi ⁇ nal water content of the plant tissue material in its fresh state, the drying of the material being performed without any substantially concomitant removal of dry matter, such as by evaporation of water.
  • the plant tissue material has a high content of pectic substances, and materials which on a dry matter basis contains more than 15% by weight
  • the method comprises the addi ⁇ tion of an inorganic or an organic acid to the plant tissue starting material in an amount sufficient to reduce the pH to 1-3, keeping the resulting mixture at a temperature and for a period of time sufficient to obtain the desired conversion of insoluble pectic substances to the water- soluble form, followed by adjusting the pH to a higher pH within the range of 3-5 by the addition of a base.
  • the crude pectin product is useful for a number of applica ⁇ tions including water absorption and/or water holding, gelling of aqueous suspensions, and as a dietary adjunct e.g. as a cholesterol-reducing agent.
  • the invention therefore relates to the use of the product as a water absorbing and/or water holding agent, as a gelling agent and as a dietary fibre additive.
  • One object of the present invention is to provide a novel inexpensive crude pectin-containing product having a dry matter content of at least 85%.
  • the term "crude” is used to describe a pectin- containing product which comprises at least all water- insoluble components of the vegetable pectin-containing starting material in which material plant tissue structures are microscopically recognizable, these components option ⁇ ally being present in the product in a modified form rela ⁇ tive to the starting material.
  • the dry matter (DM) content of the product is at least 85%.
  • the storage stability of the product will be reduced to an unacceptable level since at such lower DM contents the product will be prone to deterioration by chemical and microbiological processes.
  • products having such low water contents may absorb humidity from the surrounding atmosphere. It may therefore be necessary to provide the product of the invention in a packaging consisting of materials which are water vapour tight, e.g. plastic foils or metal foils.
  • the low water content may be maintained by the incorporation of suitable water absorbing compounds such as silica gel.
  • the product according to the inven ⁇ tion comprises 5-45% pectic substances calculated as galac- turonic acid.
  • pectic substances is used to describe the total content of polygalacturonic acid-con ⁇ taining components in the product and it includes both water-insoluble protopectin and water-soluble pectic sub- stances.
  • Protopectin is a term which is used to describe pectic substances as they occur naturally in plant materi ⁇ als. These native pectic substances are insoluble in cold water but will give rise to water-soluble pectic substances upon a variety of treatments such as heating with water, treatment with acids, or ion-exchange agents.
  • protopectin is a pectin-cellulose complex.
  • the method for determining the content of galacturonic acid is described hereinbelow.
  • the proportion of galacturonic acid in pectic substances varies according to the vegetable source and to the physiological stage of the particular plant from which the substances are derived.
  • the water-soluble pectic substances in the product have a galacturonic acid content of at least 50%. It is contemplated that the present water-insoluble protopectin has a similar content of galacturonic acid.
  • the dry matter of the product according to the invention comprises 5-45% by weight of pectic substances as defined above. It is, however, preferred that the total proportion of pectic substances in the dry matter is at least 25% by weight.
  • the final content of pectic substances in the product depends on the amount hereof present in the start ⁇ ing plant tissue material.
  • the invention is based on the findings that a treatment of plant tissue materials in which essentially all pectic substances occur as protopec ⁇ tin with acid during which a restricted amount of water is added so that the total amount of water at any stage of the treatment does not substantially exceed the water content of the plant tissue materials in their fresh state, results in a conversion of 10-80% of the water-insoluble protopec ⁇ tin to water-soluble pectic substances. It is preferred that the proportion of pectic substances in the product which is converted to the water-soluble form is at least 30% by weight, preferably at least 50% by weight, and in particular at least 50% by weight.
  • pectin-containing product is predominantly attributable to the content of pectic substances and to the physical and chemical charac ⁇ teristics thereof.
  • pectic sub- stances are predominantly composed of linear chains of D- galacturonic acid residues. In the natural state most of the carboxyl groups of these acid residues are esterified with methanol. It has long been known that the degree of esterification (DE) of pectins is a major factor in deter- mining the technological characteristics of these products and it is common to classify pectins according to their ester content.
  • DE degree of esterification
  • the DE has an effect on the water absorp ⁇ tion characteristics of dried pectic substances, e.g. when they are used as water absorbing and/or water holding materials in disposable diapers, sanitary napkins and similar products. It is generally believed that in order to be suitable as an absorbent material in the above products pectic substances must have a DE of less than 45%, prefe- rably less than 20%. It has now been found that a crude pectin product can be produced which has a high water holding capacity even if the DE is in the range of 45-90%.
  • pectic substances are used as dietary fibre preparations especial- ly when they are used with the aims of reducing the choles ⁇ terol levels. It is believed that this beneficial effect is particularly associated with highly methoxylated pectins.
  • a particularly interesting aspect of the present invention is therefore to provide a crude pectin product comprising a large proportion of highly methoxylated pectic substances.
  • the product contains pectic substances wherein the degree of esterification is in the range of 45-90%. In a preferred embodiment, the degree of esterification is at least 60%
  • the water-soluble pectic substances according to the inven ⁇ tion are characterized in that they have a galacturonic acid content of at least 50% and a content of acid and alcohol insoluble solids (AAIS) in the range of 60-90% by weight as defined as solids remaining after washing with acidic 60% isopropanol.
  • AAIS acid and alcohol insoluble solids
  • These insoluble solids comprise pectin, cellulose, and proteins.
  • AAIS is determined essentially according to the method described in Food Chemical Codex, 2nd edition, 1972, p. 580.
  • the water-soluble pectic substances of the powder has a reduced viscosity (> 7r ed) which is at least 0.050 L/g and preferably in the range of 0.250 to 0.500 L/g.
  • reduced viscosity in the present context is used as an indirect indication of the mean molecular weight. Initially the specific viscosity of a pectin solution in 1% hexameta- phosphate, pH 4.5 is determined by measuring dropping periods of the pectin solution and the buffer solution at 20°C in a falling ball viscometer (Hoeppler) .
  • the specific viscosity, ⁇ s -p is defined as: (dropping period for pectin solution/dropping period for buffer solution) - 1.
  • the reduced viscosity is defined as ⁇ S p/c (L/g) where c is the concentration of pectin.
  • the product has a pH in the range of 3-5, preferably in the range of 3.5-4.5 when a 1% aqueous suspension is measured. Within this pH range the stability of the pectin is high.
  • the crude pectin-containing product has a water holding capacity (WHC) of at least 4 g water/g.
  • WSC water holding capacity
  • the water holding capacity is defined as the amount of water which is retained per g of product when 0.5 to 1 g of product having a particle size of at the most 1.0 mm is soaked in 10 ml demineralized water at ambient tempe ⁇ rature for 30 minutes, followed by centrifugation of the soaking mixture for 10 minutes at 240 x g and measuring the amount of water retained.
  • the water holding capacity of the product depend i.a. on the particle size, the content of pectic substances, the chemical composition thereof and on the raw material source.
  • the water holding capacity is at least 9 g water/g.
  • the product produced according to the method of the invention from lemon or lime fruit peels has a WHC of 9.6-9.7. In comparison to cor- responding values for the dried raw materials this is an increase of about 60-90%.
  • the high WHC of the powder makes the product useful as a water absorbing material in e. g. disposable diapers and sanitary napkins. It is furthermore believed that a dietary fibre product is particularly suitable for reducing cholesterol levels when the WHC is high.
  • a pectin-containing product which when fed to rats in choles- terol reducing amounts for at least a period of 3 weeks results in a reduced amount of serum and liver cholesterol of the animals relative to amounts of serum and liver cholesterol of control animals fed a diet not containing the product.
  • the feeding trial is described in details in the below Example 9. As it appears from the result of this trial, both blood serum and liver cholesterol levels were reduced by more than 25% and the concentration of serum triglycerides was reduced as well. It is known from a large number of human and animal studies that water-soluble pectic substances in addition to other dietary fibre com ⁇ pounds reduce the level of blood serum cholesterol.
  • the dry matter of the product according to the invention comprises 5-15% by weight of ashes.
  • ashes in this context designates the non-combustible residue com ⁇ prising inorganic compounds which are left after combustion of the present product by placing a sample hereof overnight in a furnace preheated to 600°C.
  • the resulting ashes com ⁇ prise predominantly alkaline metal ions, alkaline earth metal ions and one or more inorganic acid residues such as sulphate, phosphate, nitrate or chloride.
  • the ash content is at least 8% by weight.
  • the total content of ashes depends on the composition of the vegetable raw materials and on the amounts of acid and base added during the production of the product.
  • the dry matter of the product according to the invention comprise 40-90% by weight of non-pectic plant tissue material.
  • the composition of this material will vary considerably depending on the source of pectin-containing plant raw material. Provided the raw material has not been subjected to a washing step prior to being used in the preparation of the crude pectin product the non-pectic plant material will comprise all non-pectic substances of the particular plant raw material such as cellulose, hemi- cellulose, starch, water-soluble carbohydrates, proteins, and organic acids. When an initial washing of the plant raw material is carried out at least part of the water-soluble substances of the plant material will be removed including water-soluble carbohydrates and organic acids.
  • the crude pectin product as defined above may be in any suitable and convenient particle size and form.
  • the product is in the form of a sub- stantially free-flowing powder consisting essentially of particles of a size of at the most 1.0 mm.
  • a method for producing a product as defined above comprises subjecting plant tissue material containing pectin substances and having microscopically recognizable plant tissue structures to conditions which will convert at least part of the water-insoluble pectic substances to water-soluble pectic substances in which substances the degree of esterification initially present in the water-insoluble pectic substances is substantially preserved, followed by drying the resulting material to a water content of 15% by weight or less and optionally comminuting the dried material to obtain the product as defined hereinbefore, without at any stage adding water in an amount which will result in a water content substantial- ly higher than the original water content of the plant tissue material in its fresh state, said original water content being at the most 90% of the plant material fresh weight, the drying of the material being performed without any substantial concomitant removal of dry matter, such as by evaporation of water.
  • Plant tissue materials which are suitable as raw materials in the practice of the invention comprise any plant materi ⁇ al which has a high content of pectic substances and which is readily accessible at a competitive price.
  • Suitable raw materials are plant tissue materials which in their dry matter contain at least 5% by weight, preferably at least 10% by weight, and in particular at least 15% by weight of pectic substances.
  • Such suitable raw materials include peel, pulp and/or rag from citrus fruits such as lemons, oranges, mandarins, limes, grapefruits, tangerines and shaddocks, apple and pear pomace, potato peel, sugar beet pulp, skin of grapes, pea pods, and carrot fibre materials.
  • citrus fruits such as lemons, oranges, mandarins, limes, grapefruits, tangerines and shaddocks, apple and pear pomace, potato peel, sugar beet pulp, skin of grapes, pea pods, and carrot fibre materials.
  • Whole fruits and vegetables such as tomatoes, quinces, mangoes, pineapples, onions, olives, wood apples, bread fruits, plums, straw ⁇ berries may also be utilized as sources of raw material.
  • raw materials for the product according to the present invention are citrus fruit peel, apple pomace and sugar beet pulp. These raw materials all have a high content of pectic substances in the form of water-insoluble protopectin. Citrus peel in which the content of protopectin is in the range of 30-35% on a dry matter basis is particularly preferred. Apple pomace and sugar beet pulp dry matters have a content of water-in ⁇ soluble pectic substances in the range of 15-20%. Other pectic substance raw materials may be selected even if their content of protopectin is less than that of the preferred raw materials, e.g. if they are available at a competitive cost. It may also be appropriate to use mix ⁇ tures of two or more plant raw materials.
  • the degree of esterifica ⁇ tion of the pectic substances is an important factor which determines the favorable properties of the resulting crude pectin product.
  • the selected raw materials therefore com ⁇ prise pectic substances in which the degree of esterifica ⁇ tion is in the range of 45-90%.
  • the degree of esterification is at least 60%.
  • the raw material may be used directly as it is obtained from the fruit or vegetable processing plants. However, it may be advantageous to carry out an initial washing with cold water to remove a substantial proportion of soluble carbohydrates, proteins, organic acids and salts.
  • the plant raw material whether it has been subjected to an initial washing or not may be dried to bring down the water content to 15% or less. The drying may be carried out at temperatures ranging from ambient temperatures to about 150°C in any convenient drying equipment known per se such as a drying oven, a fluid bed dryer or a band dryer. In the dried form, the plant tissue raw material can be stored for future use.
  • raw material from overripe fruits in which enzymatic ripening processes have liberated water-soluble pectin should be avoided since part of this pectin will be lost during an initial washing of the plant material.
  • plant material in which more extensive en ⁇ zymatic activity of pectin esterases has occurred is un ⁇ suitable as a raw material since the use hereof may result in a final product comprising pectin with a reduced degree of esterification.
  • the plant tissue raw materials may therefore advantageously be divi ⁇ ded into particles of a suitable size.
  • a suitable particle size is meant to mean one which will ensure that the subsequent processing can proceed at the desired rate.
  • Fresh material are conveniently comminu ⁇ ted in a blender or a fruit cutting machine, whereas dried raw materials may be milled, ground or crushed by means of any suitable equipment known in the art.
  • the raw materials are divided into a particle size being at the most 10 mm.
  • an inorganic or organic acid is added to the raw material in an amount sufficient to reduce the pH to a value in the range of 0-5, preferably in the range of 1-3, followed by keeping the resulting mixture at a temperature and for a period of time sufficient to obtain conversion of the desired proportion of non-soluble pectic substances to water-soluble substances.
  • the acid When comminuted fresh raw material is used the acid may advantageously be added in a concentrated form in a volume of water which does not constitute more than about 5% of the total volume of the fresh plant raw material. Alterna ⁇ tive, dried finely divided plant material may be used as the starting material. In this case the concentrated acid is preferably added after dilution in a volume of water which is substantially equivalent to the amount of water which has been removed from the plant raw material during the initial drying process.
  • the moisture contents of fresh plant materials are generally within the range of 70-90%.
  • the proportion of acid-containing water to be added to the dried material is therefore preferably in the range of about 55 to about 85% relative to the resulting total volume of rehydrated plant material.
  • the volume of con ⁇ centrated acid used when dried plant materials are used depends on the pK-value of the acid and on the concentra- tion thereof.
  • the acid volume is in the range of 1-5% of the final volume.
  • demineralized water is used to rehydrate dried plant material.
  • Useful acids may be strong inorganic acids as exemplified by, but not limited to, hydrochloric acid, sulphuric acid, phosphoric acid or nitric acid. Also strong organic acids having pK-values of less than 3.5 may be useful. Examples of such suitable organic acids are formic acid, lactic acid, malic acid and oxalic acid.
  • the organic acid may be provided by the addition to the mixture of a culture of microorganisms which can convert at least some components in the plant tissue material such as water- soluble carbohydrates to organic acids as defined above.
  • a culture of microorganisms which can convert at least some components in the plant tissue material such as water- soluble carbohydrates to organic acids as defined above.
  • useful microbial cultures are cultures of lactic acid bacteria which during fermentation produce significant amounts of lactic acid and smaller amounts of e.g. formic acid.
  • the resulting mixture is agitated, blended or kneaded while being kept at a temperature ranging from ambient temperature to about 100°C, a preferred temperature being from about 50°C to about 80°C.
  • the reaction mixture is left to stand, optionally under constant agitation, blending or kneading at the selected temperature for a period of time ranging from 1 hour to 24 hours. Any sui ⁇ table combination of temperature and time within the above indicated ranges which will lead to the desired conversion of protopectin to water-soluble pectin may be selected.
  • the conversion period necessary under the selected temperature condition will to a large extent also depend on the acid concentration and the pK-value thereof.
  • reaction conditions which result in a protopectin conversion rate resulting in the desired conversion within a reaction period shorter than 1 hour. It may be advanta ⁇ geous that the physical affection during the holding period result in a further comminution of the plant material particles.
  • the conversion procedure as defined may be carried out as batchwise treatments, but it may be preferable to set up the procedure as a continuous process, wherein the plant raw material and the acid, optionally mixed with water is fed continuously to the reaction container concurrently with a continuous removal of plant material in which the desired conversion has been attained.
  • the reaction condi ⁇ tions are selected so as to obtain the conversion of a desirable proportion of protopectin to water-soluble pectin substantially without any reduction of the initial degree of esterification.
  • the desirable resulting proportion of water-soluble pectin is within the range of 10-80%, a preferred proportion being at least 40%, and a particularly preferred proportion being at least 50%.
  • the desired conver ⁇ sion of protopectin may be obtained by alternative proce ⁇ dures including the addition of an enzyme with the ability of converting at least part of the water-insoluble pectic substances into water-soluble substances or the addition of a microorganism which under the conditions prevailing in the plant raw material is capable of producing an enzyme as defined above.
  • an enzyme with the ability of converting at least part of the water-insoluble pectic substances into water-soluble substances or the addition of a microorganism which under the conditions prevailing in the plant raw material is capable of producing an enzyme as defined above.
  • Protopectinase is an enzyme occurring naturally in fruits where it is respon ⁇ sible for the conversion of protopectin into water-soluble pectinic acids.
  • Other enzymes capable of degrading pectic substances include: pectinases such as pectin polygalacturonase and pectin depolymerases.
  • pec ⁇ tolytic enzymes are produced by several microorganisms belonging to bacteria, molds and yeasts, and some of these enzymes of microbial origin are commercially available.
  • the mixture is cooled to ambient temperature and pH is adjusted to a higher value within the range of 2.5-8, a preferred range being 3-5 by the addition of a base or a mixture of bases in an amount which is at least equivalent with the amount of added acid, whereby the resulting pH-value in the mixture is adjusted to the pre- treatment level or higher.
  • the bases are selected from alkali metal compounds such as NaOH, KOH, K 2 C0 3 , Na 2 C0 3 , or NaHC0 3 ; alkaline earth metal compounds including CaC0 3 , CaO, Ca(OH) 2 , MgO, Mg(OH) 2 , and MgC0 3 ; A1(0H) 3 ; or NH 4 0H.
  • alkali metal compounds such as NaOH, KOH, K 2 C0 3 , Na 2 C0 3 , or NaHC0 3
  • alkaline earth metal compounds including CaC0 3 , CaO, Ca(OH) 2 , MgO, Mg(OH) 2 , and MgC0 3 ; A1(0H) 3 ; or NH 4 0H.
  • magnesium and calcium com ⁇ pounds are particularly preferred.
  • the alkaline compounds may be used as solid compounds or dissolved in water. Following the addition of base the mixture is stirred until the desired pH-value is achieved uniformly herein.
  • the resulting mixture is subjected to a drying procedure.
  • the mixture may be dried as is or it may be advantageous to pre-treat the material by extrusion to pellets or other shapes.
  • the drying step is carried out in a drying oven, a band dryer, a drum dryer or a fluid-bed dryer for a period of time sufficient to reduce the moisture content of the material to at the most 15% by weight, preferably to at the most 10%, and in particular to at the most 5% by weight.
  • the drying is carried out at a temperature ranging from ambient temperature to about 150°C. It may be preferred to carry out the drying at air pressures below atmospheric pressures, whereby a relatively lower drying temperature or a comparatively shorter drying period can be used resul ⁇ ting in a more gentle treatment.
  • the resulting dried crude pectin-containing product is in the form of irregular particles, flakes, cakes or lumps, the form depending on the applied drying equipment.
  • this material is milled or ground by methods known per se in the art to a substantially free- flowing powder having a particle size of at the most 1.0 mm.
  • the crude pectin product according to the invention is useful as a water absorbing and/or water holding material, a thickening and gelling agent and as a dietary fibre additive.
  • a water absorbing and/or water holding material it may be useful as a constituent of absorbent consumer products such as dis- posable diapers and sanitary napkins.
  • the present product will be useful in essentially all product where pure pectin products are currently used, e.g. as a gelling agent in jams and jellies, confectioneries, bakery products or in frozen berries.
  • pure pectin products e.g. as a gelling agent in jams and jellies, confectioneries, bakery products or in frozen berries.
  • the crude pectin product may counteract the tendency to development of "toughness" of the product which is frequently observed when such products are frozen and thawed.
  • the crude pectin product is useful in the manufacturing of beverages, especially beve- rage product which incorporates fruit tissue ingredients.
  • fruit juice products the addition of the crude pectin product can provide an increased viscosity resulting in a juice with an improved "mouthfeel" of richness when con ⁇ sumed.
  • the present pectin product may also be useful as a thickening agent in cheese products and milk products such as sour milk products.
  • the product may be useful as a stabilizer for frozen desserts or as a thicken ⁇ ing agent in pet food products.
  • Pectin products are useful in the manufacturing of several types of pharmaceuticals. In spite of their broad applica ⁇ bility, however, relatively small amounts of pure pectin products find way into pharmaceutical use due to the high cost. It is therefore anticipated that the present low-cost pectin product may become more widely used in the phar- maceutical industry than the presently available products. Examples of potential applications are as a diarrhoea treatment product or as a demulcent in minimizing gastro ⁇ intestinal irritation when irritating substances are ad ⁇ ministered. As a dietary fibre additive the product will be useful as a hypocholesterolemic agent as it has been ex ⁇ plained hereinbefore.
  • the product will be useful for diabetic patients in their management of the blood glucose levels and for overweighed subjects as a dietary slimming product.
  • the product may be used as is or it may be used as an ingredient in speciality food products.
  • the gelling or thickening properties of the product may be utilized in a number of technical uses.
  • pectin functions well as an emulsion stabilizer for oil-in- water emulsions, e.g. in the paint industry.
  • emulsion stabilizer for oil-in- water emulsions, e.g. in the paint industry.
  • paper and textile industry it may be useful as a sizing agent.
  • the properties of the product make it potentially useful as an adjunct material in the drilling industry.
  • An amount of AAIS determined as described above represent ⁇ ing exactly 250 mg of the original unwashed sample is transferred into a 250 ml Erlenmeyer flask and moistened with 1 ml of ethanol. 100 ml of carbon dioxide free water is added. The mixture is stirred until the sample is com ⁇ pletely dissolved. The solution is titrated with 0.IN NaOH to pH 9 using a pH meter with electrode. The volume re ⁇ quired in ml is recorded as v-i (initial titre) . Ten ml of 0.5N NaOH is added and the solution is stirred vigorously for 15 minutes. Then 10 ml of 0.5N HC1 is added and the solution is stirred until pH is stable.
  • the solution is titrated with 0.1N NaOH to pH 9.
  • the volume of 0.1N NaOH required in ml is recorded as v 2 (saponification titre) .
  • the degree of esterification is calculated according to the formula 100 x v 2 (v ⁇ -M ⁇ ) .
  • the weight in mg of galacturonic acid (C5H 9 O5COOH) in the original unwashed sample is calculated according to the formula (V**L+V 2 ) x 19.41, in which V**L and v 2 are the initial titre and the saponification titre, respectively, deter ⁇ mined as described above.
  • a quantity of pectin corresponding to 90 mg pectin dry matter is weighed into a 150 ml Erlenmeyer flask together with 100 g buffer solution which is prepared by dissolving 1 g sodium hexametaphosphate in distilled water and adjust ⁇ ing the pH value to 4.5 with a few drops of 4N HCL. After a few hours of stirring the pectin is dissolved. If it is not clear the solution is filtered through a porosity 2-filter crucible. Dropping periods of the resulting pectin solution and the buffer solution, respectively are measured at 20°C in a "falling ball viscometer" (Hoeppler viscometer) .
  • Hoeppler viscometer Hoeppler viscometer
  • the specific viscosity is :
  • ⁇ 7sp (Dropping period for pectin solution/drop ⁇ ping period for buffer solution) - 1
  • the reduced viscosity is:
  • One g of sample is ashed overnight at 550°C in a furnace.
  • the crucible is cooled and a minimum volume of 2M HC1 is added to dissolve the residue.
  • the solution is transferred to a 25 ml volumetric flask and diluted with demineralized water to volume.
  • a suitable aliquot of the solution is pipetted into a 50 ml volumetric flask.
  • Ten ml of 2N nitric acid is added and the solution is heated for 2 minutes.
  • the solution is cooled and 25 ml of isopropanol and 5 ml 1.3M ammonium rhodanide is added.
  • the solution is diluted to the volume with demineralized water.
  • the absorbance is measured at 500 nm (1 cm cell) using a PYE UNICAM SPI800 spectro- photometer.
  • the Fe-content is obtained from a standard curve relating absorbance to known amounts of Fe in 50 ml solutions.
  • a 1 g sample is ashed as described above and dissolved in a minimum of 2M HC1, transferred to a 50 ml volumetric flask and diluted with demineralized water to the volume.
  • the ions were determined by ion chromatography using a DIONEXTM 4000 chromatograph equipped with a DIONEX ION PACTM cation column (CS3) for the determination of Na, K, Mg and Ca, and for the determination of S0 4 a DIONEX ION PACTM anion column (AS4) was used.
  • the paste-like mixture was spread in a thin layer on trays and dried for 16 hours at 50°C in a drying cupboard to obtain 1125 g of a product which was ground in a laboratory mill to a particle size of at the most 0.5 mm.
  • the degree of esterification of the pectic substances was determined and was found to be 62.7%.
  • the product was ground in a laboratory mill to a particle size of 0.5 mm or less.
  • degree of esterifi ⁇ cation was found to be 61.0%, the content of galacturonic acid to be 32.7% and the pH of a 1% aqueous suspension was 3.7.
  • the content of AAIS was 82.2% by weight.
  • the soluble pectin was extracted as described under materials and methods. The content hereof was found to be 26.9% by weight.
  • the water- soluble pectin had a r /re ⁇ of 0.434, a degree of esterifica ⁇ tion of 62.7% and a galacturonic acid content of 66.0% by weight.
  • the product had a content of water-soluble pectin of 26.9% by weight.
  • This content of water-soluble pectin had the following characteristics: a > ?rec ⁇ of 0.346, a degree of esterification of 65.0% and a content of galacturonic acid of 64.4%.
  • the water-soluble pectin had the following characteristics: the » ?rec ⁇ was 0.358, the degree of esterification was 65.3% and the content of galacturonic acid was 67.4%.
  • the proportion of water-soluble pectin in the product relative to the total content of pectic substances was 62.0%.
  • the product contained 30.2% by weight of water-soluble pectin with the following characteristics: a > ?rec ⁇ of 0.354, a degree of esterification of 68.9% and a galacturonic acid content of 61.8%.
  • the proportion of water-soluble pectin in the product relative to the total content of pectic substances was 55.2%.
  • AAIS* Acid and alcohol insoluble solids (cellulose, pectin, protein, etc.) which remain after washing with acid 60% isopropanol. This treatment removes soluble carbohydrates, salts and water. The proportion of water-soluble pectin in the combined product relative to the total content of pectic substances was calculated to be 61.4%.
  • mice Ten weeks old male Sprague-Dawley rats with a body weight of approximately 175-200 g were housed individually in stainless steel cages and acclimatized on a standard labo ⁇ ratory diet for 1 week before beginning the study.
  • the rats were randomized, based on body weight and placed in groups of eight to be fed either the test diet or a control diet (a cellulose diet) .
  • the test diet comprised the product from Example 7. Both diets were formulated to contain 4-5% total dietary fibres and identical amounts of proteins, fat, starch, sugars, vitamins, minerals, cholic acids and cholesterol.
  • the rats were weighed at the start of the feeding of diets. Food and water were offered ad libitum for 3 weeks.
  • the final body weights of the rats were measu ⁇ red at the end of this 3 week period, the rats were anes ⁇ thetized, and blood samples were obtained by cardiac punc ⁇ ture.
  • the livers were removed and frozen together with the plasma samples. The samples were kept at -20°C until they were analyzed.
  • Serum cholesterol measurements were based on the determina ⁇ tion of hydrogen peroxide generated by the catalytic oxida ⁇ tion of cholesterol using the Abbott VP Analyzer. Serum triglycerides were determined by measuring the decrease of the absorbance occurring when NADH is oxidized to NAD, also using the Abbott VP Analyzer. Liver cholesterol was measu ⁇ red as described by Chen & Anderson, 1979, J. Nutr. ,109, 1028-1034. The results of the study are summarized in Table 3: TABLE 3 ( olesterol-reducing Effect in Rats
  • Body weight initial (g) Body weight, final (g) Serum cholesterol ( g/dl) Serum triglycerides (mg/dl) Liver cholesterol (mg/g)
  • the gelling properties of the products obtained in Examples 6 and 7 were determined according to the IFT SAG method (Food Technology, 1959, vol. XIII, no. 9, 496-500).
  • the gel strengths of the two samples of product were:
  • the water holding capacity of the product was 4.26 g water/g of product.
  • the product had a content of water-soluble pectin of 13.8% by weight.
  • This content of water-soluble pectin had the following characteristics: a ⁇ ? re d of 0.335, a degree of esterification of 66.1% and a content of galacturonic acid of 57.9%.
  • the water holding capacity of the product was 4.70 g water/g product. After extraction of the water-soluble pectin, the content hereof in the product was found to be 15.4% by weight.
  • the characteristics of the water-soluble pectin of the product were the following:
  • the proportion of water-soluble pectin in the product relative to the total content of pectic substances was 27.6%.
  • the product contained 20.5% by weight of water-soluble pectin having the following characteristics:
  • the proportion of water-soluble pectin in the product relative to the total content of pectic substances was 40.9%.
  • the product had a content of water-soluble pectin of 24.0% by weight.
  • This content of water-soluble pectin had the following characteristics: a » ?r ed of 0.340, a degree of esterification of 63.7% and a content of galacturonic acid of 59.3%.
  • the proportion of water-soluble pectin in the product relative to the total content of pectic substances was 49.8%.
  • the viscosity of the resulting pectin product was measured by means of a Haake Viscotester according to the method described above. These viscosity measurements the results of which are also indicative of the solubility of the pectin product were carried out with the pectin product as such and with the same amount of pectin product in the presence of varying amounts of the following phos- phates (P) : sodium hexametaphosphate (A) , disodium phos ⁇ phate (B) and tetrasodium pyrophosphate (C) . The amounts of the phosphates were as follows (% by weight relative to the amount of pectin product): 2, 5, 10, 15, 25, 50 and 100. The results are summarized in the below table: TABLE 4
  • the gelling properties of the product obtained in the present Example were determined according to the IFT SAG method (Food Technology. 1959, vol. XIII, no. 9, 496-500) without and in the presence of 10% by weight of sodium hexametaphosphate relative to the amount of pectin product.
  • the gel strengths of the two samples of product were: Product without phosphate SAG 0 29 Product with phosphate SAG 0 53
  • DIMODAN PMTM Hydrate is a monoglyceride additive based on tallow or lard (Grindsted Products)
  • PANODANTM 80 is an emulsifying additive comprising diacetyl tartaric acid ester of monoglycerides and diglycerides and 20% by weight CaC0 3 as an anticaking agent (Grindsted Products)
  • GRIN ⁇ DAMYLTM A 1000 is an Aspergillus oryzae ⁇ -amylase product) .
  • SOBALGTM FD 155 is a sodium alginate product (100%) from Grindsted Products.
  • 1800 g batches of buns were prepared by mixing the ingredi- ents in a TweedyTM mixing apparatus without vacuum for about 1 minute.
  • the resulting dough the temperature of which reached about 28°C rested for 5 minutes at room temperature prior to moulding using a FortunaTM moulder followed by proofing the moulded bun dough for 60 minutes at 40°C and 85% RH and baking at 220°C for 10 minutes.
  • the baked buns were tested according to standard procedures for (1) volume (cm 3 /g) and for (2) consistency after freez ⁇ ing at -20°C for 24 hours and thawing in a microwave oven for about 30 seconds at 500 W.
  • volume values were as follows: recipe no. 1 (control) : 7.5; recipe no. 2 (control with added alginate): 5.9; recipe no 3: 7.0; recipe no. 4: 6.9.
  • a batch of strawberry jam was prepared according to the following recipe:
  • Citric acid 50% (w/v) 0.90% Total 113.15%
  • the pectin product and the hexametaphosphate were added to about 80°C hot water in a high speed mixer.
  • the strawber- ries and sugar were mixed and brought to the boil.
  • the pectin product solution was added to the fruit/sugar mix ⁇ ture and boiling was continued until a level of soluble solids (SS) of 65% was reached and finally, the citric acid was added.
  • the resulting jam had a pH of 3.1.
  • the gelling of the jam was characterized by measuring the internal strength of the gel by means of a Voland Stevens Texture Analyser as described by Ikkala (Proceedings of the Third International Conference and Industrial Exhibition, North East Wales Institute, Wrexham. U.K.. 1985, 3-15) . Using a plunger velocity of 0.5 mm/second and a penetration of 10 mm an internal strength value of 47 g was measured. This confirms that the crude pectin product is useful as a gelling agent in fruit jams, in particular in the presence of a phosphate. By varying the amounts of the crude pectin product and the phosphate it is possible to obtain a desi- red gelling of fruit jams.
  • pectin jellies In the manufacturing of the confectionery product, pectin jellies the desired gel strength is obtained by the incor ⁇ poration of highly purified pectin products. Experiments were carried out to study the usefulness of the present crude pectin product as a gelling agent in pectin jellies. The following recipe was selected:
  • Citric acid was dissolved in water at 70°C.
  • the pectin product and the phosphate were added to this solution under vigorous agitation.
  • the sugar and syrup ingredients were heated to boiling and the pectin product-containing solu ⁇ tion was added hereto and boiling continued until a level of soluble solids of 78% had been reached by evaporation.
  • Finally the resulting mixture was transferred to moulds and left for setting for about 24 hours.
  • the resulting pectin jellies had an acceptable texture and reasonable gel strength indicating that the crude pectin product may be a useful gelling agent in gelled confec ⁇ tionery products such as pectin jellies.
  • Purified pectin products are frequently used as ingredients in fruit juices in order to provide a desired viscosity in the juice resulting in a mouthfeel of "richness". Experi- ments were carried out to evaluate whether the crude pectin product can replace purified pectins as the viscosity increasing agent in fruit juices. As an example a batch of orange juice was prepared according to the following reci ⁇ pe:
  • the resulting ready-to-use orange juice had a mouthfeel which was comparable to that of an orange juice containing a purified pectin product (MEXPECTINTM RS 461, Grindsted Products) as the viscosity increasing agent.

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Abstract

Nouveau produit végétal économique, contenant de la pectine brute, préparé à partir de déchets agricoles et procédé de fabrication. Le produit comprend de 5 à 45 % de substances pectiques dont 25 % au moins se présentent sous forme soluble dans l'eau. Les substances pectiques contenues dans ce produit possèdent un degré d'estérification situé dans une gamme de 45-90 %. Ce produit est efficace comme agent épaississant et gélifiant, agent d'absorption aqueuse et additif de fibres diététiques, particulièrement pour abaisser les taux de cholestérol dans le sang.
PCT/DK1991/000072 1990-03-30 1991-03-08 Produit contenant de la pectine et procede de fabrication WO1991015517A1 (fr)

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DK081690A DK81690D0 (da) 1990-03-30 1990-03-30 Pektinprodukt og fremgangsmaade til fremstilling deraf
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Cited By (30)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2253984A (en) * 1991-03-25 1992-09-30 Assutech Ltd Edible composition
EP0542353A1 (fr) * 1991-11-14 1993-05-19 Unilever N.V. Pâtons fermentés surgelés
US5304374A (en) * 1989-10-30 1994-04-19 Humanetics Corporation Process for enhancing the hypocholesterolemic effect of edible pulp and the product obtained thereby
US5354851A (en) * 1993-03-31 1994-10-11 Humanetics Corporation Process for producing crude pectin through ion exchange
US5403612A (en) * 1993-03-31 1995-04-04 Humanetics Corporation Process for producing a phosphorylated pectin-containing fiber product
US5567462A (en) * 1992-02-06 1996-10-22 Sanofi Bio-Industries, Inc. Pecto-cellulosic product from whole citrus peel and other materials
US5656734A (en) * 1995-10-30 1997-08-12 Systems Bio-Industries Methods for making pectin and pectocellulosic products
WO1998002488A1 (fr) * 1996-07-12 1998-01-22 Norsk Hydro Asa Utilisation de polysaccharides du bloc g
US5968927A (en) * 1996-09-20 1999-10-19 Idun Pharmaceuticals, Inc. Tricyclic compounds for the inhibition of the ICE/ced-3 protease family of enzymes
KR100258584B1 (ko) * 1997-10-28 2000-07-01 박호군 감귤류과피추출액을포함하는아실코에이:콜레스테롤-오르토-아실트랜스퍼레이즈저해제조성물
US6221419B1 (en) 1998-11-05 2001-04-24 Hercules Incorporated Pectin for stabilizing proteins
FR2813010A1 (fr) * 2000-08-16 2002-02-22 Aurore Dev S A Procede de fabrication d'un extrait d'argrumes riche en pectine, et extrait obtenu par ce procede
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
WO2003009705A1 (fr) * 2001-07-25 2003-02-06 Südzucker Aktiengesellschaft Sucre de gelification et procede de fabrication
US6699977B1 (en) 2000-06-09 2004-03-02 Cp Kelco Aps Low methoxyl pectins, processes thereof, and stabilized aqueous systems comprising the same
WO2004020472A2 (fr) * 2002-09-02 2004-03-11 Cp Kelco Aps Procede ameliore pour traiter de la matiere vegetale contenant de la pectine
EP1745705A1 (fr) * 2005-07-20 2007-01-24 N.V. Nutricia Procédé de préparation d' oligosaccharides d' acide uronique par extrusion
US7371402B2 (en) 1998-08-14 2008-05-13 Danisco A/S Use of a composition
WO2009019088A1 (fr) 2007-08-03 2009-02-12 Nestec S.A. Système de stabilisateur naturel pour dessert glacé
US7648720B2 (en) 1995-12-26 2010-01-19 Cns, Inc. Dietary fiber delivery system
EP2196242A1 (fr) 2004-04-26 2010-06-16 CP Kelco ApS Composition de controle de l'alcalinite et de protection pour la peau et son utilisation
US8592575B2 (en) 2011-06-06 2013-11-26 Cp Kelco Aps Process for extraction of pectin
EP3187511A4 (fr) * 2014-08-28 2018-01-24 Fuji Oil Holdings Inc. Procédé de production d'un polysaccharide de pois soluble dans l'eau
US20190159494A1 (en) * 2016-07-08 2019-05-30 Cargill, Incorporated Dispersion containing citrus fibers
US10667543B2 (en) 2014-12-22 2020-06-02 Conopco, Inc. Frozen confection
WO2020225116A1 (fr) * 2019-05-07 2020-11-12 Société des Produits Nestlé S.A. Composition d'aliment ou de boisson en poudre
EP3466983B1 (fr) 2017-02-15 2021-07-14 CP Kelco ApS Compositions de biomasse contenant de la pectine activée, produits et procédés de production
CN114634655A (zh) * 2022-03-24 2022-06-17 重庆檬泰生物科技有限公司 一种用于益生菌包被的果胶生产工艺
WO2022261116A1 (fr) * 2021-06-08 2022-12-15 Corn Products Development, Inc. Fibres d'agrumes gélifiantes et procédés de fabrication
US11987650B2 (en) 2017-02-15 2024-05-21 Cp Kelco Aps Activated pectin-containing biomass compositions and products

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DE4011285A1 (de) * 1990-04-06 1991-10-10 Steigerwald Arzneimittelwerk Arzneimittel zur behandlung von hyperlipidaemie und/oder atherosklerose
AU651626B2 (en) * 1990-10-24 1994-07-28 Nestec S.A. Medical foods having soluble fiber

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GB472974A (en) * 1935-04-01 1937-10-01 Fruit Growers Exchange Ca Process of treating vegetable matter containing protopectin
US2452750A (en) * 1941-09-03 1948-11-02 Halliday Supplemental therapeutic food
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US5304374A (en) * 1989-10-30 1994-04-19 Humanetics Corporation Process for enhancing the hypocholesterolemic effect of edible pulp and the product obtained thereby
GB2253984B (en) * 1991-03-25 1995-03-22 Assutech Ltd Edible composition
GB2253984A (en) * 1991-03-25 1992-09-30 Assutech Ltd Edible composition
EP0542353A1 (fr) * 1991-11-14 1993-05-19 Unilever N.V. Pâtons fermentés surgelés
US5567462A (en) * 1992-02-06 1996-10-22 Sanofi Bio-Industries, Inc. Pecto-cellulosic product from whole citrus peel and other materials
US5354851A (en) * 1993-03-31 1994-10-11 Humanetics Corporation Process for producing crude pectin through ion exchange
US5403612A (en) * 1993-03-31 1995-04-04 Humanetics Corporation Process for producing a phosphorylated pectin-containing fiber product
US5656734A (en) * 1995-10-30 1997-08-12 Systems Bio-Industries Methods for making pectin and pectocellulosic products
US7648720B2 (en) 1995-12-26 2010-01-19 Cns, Inc. Dietary fiber delivery system
WO1998002488A1 (fr) * 1996-07-12 1998-01-22 Norsk Hydro Asa Utilisation de polysaccharides du bloc g
AU713991B2 (en) * 1996-07-12 1999-12-16 Fmc Biopolymer As Use of G-block polysaccharides
US6187771B1 (en) 1996-09-20 2001-02-13 Idun Pharmaceuticals, Inc. Tricyclic compounds for the inhibition of the ICE/ced-3 protease family of enzymes
US5968927A (en) * 1996-09-20 1999-10-19 Idun Pharmaceuticals, Inc. Tricyclic compounds for the inhibition of the ICE/ced-3 protease family of enzymes
US6444663B2 (en) 1996-09-20 2002-09-03 Idun Pharmaceuticals, Inc. Tricyclic compounds for the inhibition of the ICE/ced-3 protease family of enzymes
KR100258584B1 (ko) * 1997-10-28 2000-07-01 박호군 감귤류과피추출액을포함하는아실코에이:콜레스테롤-오르토-아실트랜스퍼레이즈저해제조성물
US7371402B2 (en) 1998-08-14 2008-05-13 Danisco A/S Use of a composition
US6221419B1 (en) 1998-11-05 2001-04-24 Hercules Incorporated Pectin for stabilizing proteins
US6699977B1 (en) 2000-06-09 2004-03-02 Cp Kelco Aps Low methoxyl pectins, processes thereof, and stabilized aqueous systems comprising the same
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
FR2813010A1 (fr) * 2000-08-16 2002-02-22 Aurore Dev S A Procede de fabrication d'un extrait d'argrumes riche en pectine, et extrait obtenu par ce procede
CZ305243B6 (cs) * 2001-07-25 2015-07-01 SĂśDZUCKER AKTIENGESELLSCHAFT MANNHEIM/OCHSENFURT Želírovací kompozice, použití této želírovací kompozice, přípravek obsahující tuto želírovací kompozici, způsob výroby tohoto přípravku a zařízení k provádění tohoto způsobu
WO2003009705A1 (fr) * 2001-07-25 2003-02-06 Südzucker Aktiengesellschaft Sucre de gelification et procede de fabrication
WO2004020472A2 (fr) * 2002-09-02 2004-03-11 Cp Kelco Aps Procede ameliore pour traiter de la matiere vegetale contenant de la pectine
WO2004020472A3 (fr) * 2002-09-02 2004-04-01 Cp Kelco Aps Procede ameliore pour traiter de la matiere vegetale contenant de la pectine
EP2196242A1 (fr) 2004-04-26 2010-06-16 CP Kelco ApS Composition de controle de l'alcalinite et de protection pour la peau et son utilisation
EP1745705A1 (fr) * 2005-07-20 2007-01-24 N.V. Nutricia Procédé de préparation d' oligosaccharides d' acide uronique par extrusion
WO2007009776A1 (fr) 2005-07-20 2007-01-25 N.V. Nutricia Procede de preparation d'oligosaccharides d'acide uronique par extrusion
WO2009019088A1 (fr) 2007-08-03 2009-02-12 Nestec S.A. Système de stabilisateur naturel pour dessert glacé
EP2025240A1 (fr) * 2007-08-03 2009-02-18 Nestec S.A. Système de stabilisateur naturel pour dessert glacé
US8956680B2 (en) 2007-08-03 2015-02-17 Nestec S.A. Natural stabiliser system for frozen dessert
US8592575B2 (en) 2011-06-06 2013-11-26 Cp Kelco Aps Process for extraction of pectin
EP3187511A4 (fr) * 2014-08-28 2018-01-24 Fuji Oil Holdings Inc. Procédé de production d'un polysaccharide de pois soluble dans l'eau
US10667543B2 (en) 2014-12-22 2020-06-02 Conopco, Inc. Frozen confection
US20190159494A1 (en) * 2016-07-08 2019-05-30 Cargill, Incorporated Dispersion containing citrus fibers
EP3466983B1 (fr) 2017-02-15 2021-07-14 CP Kelco ApS Compositions de biomasse contenant de la pectine activée, produits et procédés de production
US11987650B2 (en) 2017-02-15 2024-05-21 Cp Kelco Aps Activated pectin-containing biomass compositions and products
WO2020225116A1 (fr) * 2019-05-07 2020-11-12 Société des Produits Nestlé S.A. Composition d'aliment ou de boisson en poudre
WO2022261116A1 (fr) * 2021-06-08 2022-12-15 Corn Products Development, Inc. Fibres d'agrumes gélifiantes et procédés de fabrication
CN114634655A (zh) * 2022-03-24 2022-06-17 重庆檬泰生物科技有限公司 一种用于益生菌包被的果胶生产工艺

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AR245735A1 (es) 1994-02-28
IL97528A0 (en) 1992-06-21
ZA911903B (en) 1992-01-29
MX25011A (es) 1993-12-01
AU7554591A (en) 1991-10-30

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