WO2014064591A1 - Microencapsulation au moyen de protéines de légume - Google Patents

Microencapsulation au moyen de protéines de légume Download PDF

Info

Publication number
WO2014064591A1
WO2014064591A1 PCT/IB2013/059458 IB2013059458W WO2014064591A1 WO 2014064591 A1 WO2014064591 A1 WO 2014064591A1 IB 2013059458 W IB2013059458 W IB 2013059458W WO 2014064591 A1 WO2014064591 A1 WO 2014064591A1
Authority
WO
WIPO (PCT)
Prior art keywords
microcapsules
microcapsule
oil
maltodextrin
encapsulated
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.)
Ceased
Application number
PCT/IB2013/059458
Other languages
English (en)
Inventor
Michael T. NICKERSON
Nicholas Low
Asli CAN KARACA
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.)
University of Saskatchewan
Original Assignee
University of Saskatchewan
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 University of Saskatchewan filed Critical University of Saskatchewan
Publication of WO2014064591A1 publication Critical patent/WO2014064591A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/02—Making microcapsules or microballoons
    • B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23B—PRESERVATION OF FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES; CHEMICAL RIPENING OF FRUIT OR VEGETABLES
    • A23B2/00—Preservation of foods or foodstuffs, in general
    • A23B2/90—Preservation of foods or foodstuffs, in general by drying or kilning; Subsequent reconstitution
    • A23B2/92—Freeze drying
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS OR COOKING OILS
    • A23D9/00—Other edible oils or fats, e.g. shortenings or cooking oils
    • A23D9/007—Other edible oils or fats, e.g. shortenings or cooking oils characterised by ingredients other than fatty acid triglycerides
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23G—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF
    • A23G9/00—Frozen sweets, e.g. ice confectionery, ice-cream; Mixtures therefor
    • A23G9/32—Frozen sweets, e.g. ice confectionery, ice-cream; Mixtures therefor characterised by the composition containing organic or inorganic compounds
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23G—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF
    • A23G9/00—Frozen sweets, e.g. ice confectionery, ice-cream; Mixtures therefor
    • A23G9/32—Frozen sweets, e.g. ice confectionery, ice-cream; Mixtures therefor characterised by the composition containing organic or inorganic compounds
    • A23G9/327—Frozen sweets, e.g. ice confectionery, ice-cream; Mixtures therefor characterised by the composition containing organic or inorganic compounds characterised by the fatty product used, e.g. fat, fatty acid, fatty alcohol, their esters, lecithin, glycerides
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23G—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF
    • A23G9/00—Frozen sweets, e.g. ice confectionery, ice-cream; Mixtures therefor
    • A23G9/32—Frozen sweets, e.g. ice confectionery, ice-cream; Mixtures therefor characterised by the composition containing organic or inorganic compounds
    • A23G9/38—Frozen sweets, e.g. ice confectionery, ice-cream; Mixtures therefor characterised by the composition containing organic or inorganic compounds containing peptides or proteins
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23G—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF
    • A23G9/00—Frozen sweets, e.g. ice confectionery, ice-cream; Mixtures therefor
    • A23G9/44—Frozen sweets, e.g. ice confectionery, ice-cream; Mixtures therefor characterised by shape, structure or physical form
    • A23G9/48—Composite products, e.g. layered, laminated, coated, filled
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23J—PROTEIN COMPOSITIONS FOR FOODSTUFFS; WORKING-UP PROTEINS FOR FOODSTUFFS; PHOSPHATIDE COMPOSITIONS FOR FOODSTUFFS
    • A23J1/00—Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites
    • A23J1/14—Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites from leguminous or other vegetable seeds; from press-cake or oil-bearing seeds
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23J—PROTEIN COMPOSITIONS FOR FOODSTUFFS; WORKING-UP PROTEINS FOR FOODSTUFFS; PHOSPHATIDE COMPOSITIONS FOR FOODSTUFFS
    • A23J3/00—Working-up of proteins for foodstuffs
    • A23J3/14—Vegetable proteins
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/115—Fatty acids or derivatives thereof; Fats or oils
    • A23L33/12—Fatty acids or derivatives thereof
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P10/00—Shaping or working of foodstuffs characterised by the products
    • A23P10/30—Encapsulation of particles, e.g. foodstuff additives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/02—Making microcapsules or microballoons
    • B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
    • B01J13/043—Drying and spraying
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23C—DAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; PREPARATION THEREOF
    • A23C13/00—Cream; Cream preparations; Making thereof
    • A23C13/12—Cream preparations
    • A23C13/16—Cream preparations containing, or treated with, microorganisms, enzymes, or antibiotics; Sour cream
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23C—DAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; PREPARATION THEREOF
    • A23C9/00—Milk preparations; Milk powder or milk powder preparations
    • A23C9/12—Fermented milk preparations; Treatment using microorganisms or enzymes
    • A23C9/13—Fermented milk preparations; Treatment using microorganisms or enzymes using additives
    • A23C9/1307—Milk products or derivatives; Fruit or vegetable juices; Sugars, sugar alcohols, sweeteners; Oligosaccharides; Organic acids or salts thereof or acidifying agents; Flavours, dyes or pigments; Inert or aerosol gases; Carbonation methods
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23C—DAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; PREPARATION THEREOF
    • A23C9/00—Milk preparations; Milk powder or milk powder preparations
    • A23C9/152—Milk preparations; Milk powder or milk powder preparations containing additives
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs

Definitions

  • Some embodiments of the present invention relate to methods and compositions for the preservation and/or improvement of materials by microencapsulation. Some embodiments of the present invention relate to methods and compositions for the preservation and/or improvement of oils by microencapsulation. Some embodiments of the present invention relate to methods and compositions for the preservation and/or improvement of oils rich in polyunsaturated fatty acids by microencapsulation.
  • Flaxseed oil is rich in essential fatty acids including polyunsaturated fatty acids (PUFA) such as a-linolenic acid, which are purported to induce a variety of health benefits upon consumption. These health benefits include: reducing the risk of coronary heart diseases (Li, Attar-Bashi & Sinclair, 2003), protection against inflammation (Bloedon, L. T. et al., 2008), and the prevention of breast and prostate cancers (Bougnoux & Chajes, 2003).
  • PUFA polyunsaturated fatty acids
  • flaxseed oil remains underutilized by the food industry due to its susceptibility to oxidation because of its high PUFA content, distinct taste, and lack of miscibility in aqueous food systems (Lukaszewicz, Szopa & Krasowska, 2004; Bozan & Temelli, 2008).
  • these limitations can potentially be circumvented so as to offer PUFA protection to the harsh environmental conditions experienced during food processing and storage, and to improve flaxseed oil miscibility in foods and mask its distinct taste.
  • flaxseed oil is rich in polyunsaturated fatty acids (PUFAs), it is highly susceptible to oxidation resulting in the onset of rancidity.
  • Lukaszewicz, Szopa & Krasowska (2004) investigated the oxidative stability of flaxseed oil produced from nine different cultivars by measuring both conjugated dienes and 2-thiobarbituric acid-reactive substances (TBARS) formation following sample storage in air at 140°C for 40 min. Results from these experiments showed that the concentration of conjugated dienes reached 50-200 mol/kg, whereas TBARS reached 0.1-0.5 mol/kg. Based on these results, the authors concluded that flaxseed oil isolated from all nine cultivars was easily oxidized.
  • PUFAs polyunsaturated fatty acids
  • Encapsulation is defined as a process whereby an active ingredient becomes enclosed or packaged within micron-sized carrier matrices, which in turn segregates and protects the inner core from the surrounding environment (Gibbs, Kermasha, Alii & Mulligan, 1999).
  • the particle size of the active ingredient (e.g. oil) dispersed within the aqueous phase of the emulsion has been shown to be a significant factor for retention within microcapsules, where the smaller the particle size the greater the retention (Rish and Reineccius, 1988). Smaller oil droplet sizes have also been shown to minimize microcapsule surface oil, increase oil encapsulation efficiency and decrease lipid oxidation rates (Lee & Ying, 2008).
  • gelatin is one of the most widely used encapsulating materials it suffers from a number of perceived safety concerns (e.g., prion disease), and religious and dietary restrictions. Therefore, the development of plant protein based encapsulation systems as an alternative to animal proteins is of considerable interest and importance.
  • Legume proteins can serve as a potential source for this purpose because of their high nutritional value, low cost and purported beneficial health benefits including but not limited to, reducing the risk of cardiovascular disease, as an aid in glycemic control in diabetic individuals, and in the prevention of digestive tract diseases (Boye et al., 2010; Duranti, 2006).
  • the major storage proteins in legume seeds are globulins and albumins. Globulins represent -70% of the protein found in legume seeds and are classified as either 1 IS (legumins; S - Svedberg Unit) or 7S (vicilins) based on their sedimentation coefficients (Roy et al., 2010).
  • Legumin is a hexameric protein with an overall molecular weight of 300-400 kDa whereas vicilin is a trimeric protein with a molecular weight between 150-180 kDa (Derbyshire et al., 1976).
  • Albumins constitute 10-20% of the protein in legume seeds and can have variable molecular weights (16-483 kDa) (Papalamprou et al., 2010).
  • Maltodextrins are widely used as wall materials for capsule formation as they exhibit good solubility and low viscosities at high solids contents (Gharsallaoui et al., 2007). Maltodextrin can be used as a secondary wall material (i.e., filler) to improve microcapsule drying properties (Kagami et al., 2003; Bae and Lee, 2008).
  • freeze drying is a dehydration process whereby an emulsion is initially frozen, then put on under pressure in a vacuum to allow the ice to sublimate from a solid to a gas.
  • Fluidized bed coating is a process whereby a pressurized emulsion is introduced to a solid secondary wall material (e.g., maltodextrin). The solid/fluid mixture behaves as a fluid within the drying bed to ensure excellent heat transfer.
  • Spray chilling can also be used to produce microcapsules.
  • Spray drying is a common step used in the production of microencapsulated food ingredients (Pegg & Shahidi, 2007).
  • Spray-drying involves the atomization of an emulsion into a wall material (e.g., whey protein isolate, gum Arabic, maltodextrin, etc.) under a hot air current, resulting in rapid water evaporation and instantaneous entrapment of the core material (Gharsallaoui et al., 2007).
  • a wall material e.g., whey protein isolate, gum Arabic, maltodextrin, etc.
  • a microcapsule has a core of a material to be encapsulated and a shell comprising a legume protein and a low molecular weight carbohydrate.
  • the material to be encapsulated is an oil.
  • the oil is an oil rich in polyunsaturated fatty acids.
  • the oil is rich in omega-3 fatty acids, a-linolenic acid, eicosapentaenoic acid (EPA), and/or docosahexaenoic acid (DHA).
  • the material to be encapsulated is flaxseed oil, fish oil, flavour oil, fragrance oil, and/or an oil-soluble vitamin.
  • the legume protein is chickpea protein, lentil protein, faba bean protein, or soybean protein.
  • the low molecular weight carbohydrate is dextrin or glycose syrup solids. In some embodiments, the dextrin is maltodextrin.
  • the amount of legume protein in an emulsion from which the microcapsule is prepared is between about 3% and about 10% w/v. In some embodiments, the amount of low molecular weight carbohydrate in an emulsion from which the microcapsule is prepared is between about 20% w/v to about 50% w/v. In some embodiments, the amount of material to be encapsulated in an emulsion from which the microcapsule is prepared is in the range of about 5% w/v to about 25% w/v.
  • the microcapsules are incorporated into a food product.
  • the food product is a dairy product or a dry food product.
  • the food product has a relatively neutral pH, for example, between about 6.5 and 7.0.
  • a method for producing microcapsules includes combining a material to be encapsulated, a legume protein and a low molecular weight carbohydrate, mixing the resultant solution to form an emulsion, and forming microcapsules.
  • forming microcapsules comprises spray drying, freeze drying, spray chilling, or fluidized bed coating.
  • the microcapsules are incorporated in a food product to provide delayed release of the encapsulated material. In some embodiments, the microcapsules are incorporated in a food product to provide delivery of the encapsulated material to the gastrointestinal tract of an animal, including a human. In some
  • the microcapsules are incorporated in a food product to hide the taste of the encapsulated material.
  • the microcapsules are formed to enhance the miscibility of the material encapsulated in the microcapsules in a food product.
  • Figure 4 shows SEM images of freeze-dried CPI- and LPI-based microcapsules produced at conditions of 10.5% flaxseed oil and 35.5% maltodextrin-DE 9: a) CPI at pH 3.0; b) LPI at pH 3.0; c) CPI at pH 7.0; d) LPI at pH 7.0.
  • PV peroxide value
  • TBARS thiobarbituric acid- reactive substances
  • Figure 7 shows SEM images of spray-dried flaxseed oil microcapsules containing: a) CPI and 10% oil; b) CPI and 15% oil; c) CPI and 20% oil; d) LPI and 10% oil; e) LPI and 15% oil; f) LPI and 20% oil.
  • microcapsules having a core of material to be encapsulated and a shell comprising a legume protein and a low molecular weight carbohydrate.
  • such microcapsules are used to protect the material to be encapsulated, e.g. from oxidation or degradation, and/or to improve the properties of the material to be encapsulated, e.g. to facilitate delayed or gradual release of the material to be encapsulated, e.g. for use in a product consumed orally by a human or other animal, or to hide the taste of the material to be encapsulated from the human or other animal.
  • the material to be encapsulated is an oil.
  • the material to be encapsulated is an oil rich in polyunsaturated fatty acids.
  • the material to be encapsulated is an oil rich in omega-3 fatty acids, such as eicosapentaenoic acid (EPA) or docosahexaenoic acid (DHA), such as a fish oil.
  • the material to be encapsulated is an oil rich in a- linolenic acid, such as flaxseed oil.
  • the material to be encapsulated is a flavour oil, fragrance oil, oil-soluble vitamin, or the like.
  • the legume protein is chickpea protein or lentil protein. In some embodiments, the legume protein is faba bean protein or soybean protein. The preparation of stable emulsions of chickpea, faba bean, lentil and soy protein isolates has been previously described (Can Karaca et al., 2011). In some embodiments, the legume protein is chickpea protein isolate or lentil protein isolate.
  • the low molecular weight carbohydrate is dextrin, i.e. a low molecular weight carbohydrate produced by the hydrolysis of starch or glycogen. In some embodiments, the low molecular weight carbohydrate is maltodextrin.
  • the low molecular weight carbohydrate is maltodextrin-DE 9 or maltodextrin-DE 18. In some embodiments, the low molecular weight carbohydrate is maltodextrin-DE 3, maltodextrin-DE 4, maltodextrin-DE 5, maltodextrin-DE 6, maltodextrin-DE 7, maltodextrin-DE 8, maltodextrin-DE 9, maltodextrin-DE 10, maltodextrin-DE 11, maltodextrin-DE 12, maltodextrin-DE 13, maltodextrin-DE 14, maltodextrin-DE 15, maltodextrin-DE 16, maltodextrin-DE 17, maltodextrin-DE 18, maltodextrin-DE 19, or maltodextrin-DE 20. In some embodiments, the low molecular weight carbohydrate is a combination of two or more of the foregoing maltodextrins. In some embodiments, the low molecular weight
  • methods for preparing microcapsules having a core of material to be encapsulated and a shell comprising a legume protein and a low molecular weight carbohydrate are provided.
  • legume protein isolates are dissolved in aqueous solution
  • the low molecular weight carbohydrate is dissolved in aqueous solution
  • the dissolved low molecular weight carbohydrate and legume protein isolates are combined with the material to be encapsulated.
  • the pH of any of the solutions, including the legume protein isolate solution is optionally adjusted to any desired pH.
  • the pH of the lentil protein isolate solution is adjusted to 3.0 or 7.0 prior to its addition to the low molecular weight carbohydrate and the material to be encapsulated.
  • the resulting solution is mixed to form an emulsion solution.
  • mixing the resulting solution includes homogenizing the solution. Any suitable equipment may be used to homogenize the solution, for example, homogenizers, including e.g. high pressure valve homogenizers.
  • the emulsion solution is then processed in any suitable manner to produce microcapsules, for example by freeze drying, spray drying, fluidized bed coating, spray chilling, or the like.
  • the amount of legume protein in the emulsion solution is in the range of about 3% to about 10% w/v or any value therebetween, e.g. 4%, 5%, 6%, 7%, 8% or 9%. In some embodiments, the amount of legume protein in the emulsion solution is about 4% w/v.
  • the amount of low molecular weight carbohydrate in the emulsion solution is in the range of about 20% w/v to about 50% w/v, or any value therebetween, e.g. 22%, 24%, 26%, 28%, 30%, 32%, 34%, 36%, 38%, 40%, 42%, 44%, 46% or 48% w/v. In some embodiments, the amount of low molecular weight carbohydrate is in the range of about 30% to about 40% w/v.
  • the amount of material to be encapsulated in the emulsion solution is in the range of about 5% w/v to about 25% w/v, or any value therebetween, e.g. 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, 20%, 21%, 22%, 23% or 24% w/v.
  • the amount of material to be encapsulated in the emulsion solution is in the range of about 10% to about 20% w/v. Decreasing the amount of material to be encapsulated in the emulsion solution can increase the encapsulation efficiency and result in lower surface oil content in the resultant microcapsules.
  • the amount of material to be encapsulated in the microcapsules is in the range of about 10% w/w to about 20% w/w or any value therebetween, e.g. 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18% or 19% w/w.
  • microcapsules are used to provide the material to be encapsulated in a form suitable for use in food products.
  • Microencapsulation can be used for many purposes; for example, to protect the material to be encapsulated from oxidation, to hide the taste of the material to be encapsulated from a person or other organism consuming the food product, to allow for delayed release of the material to be encapsulated after consumption of the food product, and/or to render the material to be encapsulated miscible in the food product.
  • the food product has a relatively neutral pH.
  • the food product is a dairy product, for example, milk, cheese, yogurt, sour cream, ice cream or the like.
  • the food product is a dry product such as cereals, granola bars, or the like.
  • the dry food product has a relatively neutral pH, e.g. a pH of approximately 6.5 to 7.0.
  • the food product is animal feed.
  • microcapsules are added to feed to potentially increase the transfer of oils (containing essential fatty acids including omega-3 fatty acids) through the animal (for example, dairy cows, beef cows, chickens or other livestock) to give omega-3 fatty acid-rich products (for example, milk, meat and eggs that are higher in omega-3 fatty acid content than equivalent product obtained from animals not fed animal feed including microcapsules containing oils high in desirable fatty acids such as omega-3 fatty acids).
  • oils containing essential fatty acids including omega-3 fatty acids
  • omega-3 fatty acid-rich products for example, milk, meat and eggs that are higher in omega-3 fatty acid content than equivalent product obtained from animals not fed animal feed including microcapsules containing oils high in desirable fatty acids such as omega-3 fatty acids.
  • the microcapsules would in principle protect the oil within the feed and within the gastrointestinal tract of the animal from oxidation and/or degradation.
  • the amount of material to be encapsulated that is released from the microcapsules at a relatively neutral pH is relatively low, e.g. less than about 10%, less than about 9%, less than about 8%, less than about 7%, less than about 6% or less than about 5% of the encapsulated material is released at a relatively neutral pH of between about 6.0 and about 8.0 or any value therebetween, e.g. a pH of 6.2, 6.4, 6.6, 6.8, 7.0, 7.2, 7.4, 7.6 or 7.8.
  • the amount of material to be encapsulated that is released from the microcapsules under gastric conditions e.g. as would be experienced in the stomach of an animal that has consumed the microcapsules (e.g. a pH of 1.2 with pepsin present in the human stomach), and/or the amount of material released from the microcapsules under intestinal conditions, e.g. as would be experienced in the intestine of an animal that has consumed the microcapsules (e.g. a pH of 6.8 in the presence of pancreatin in the human intestine) is relatively high, e.g. greater than about 30%, greater than about 40%, greater than about 50%, greater than about 60%, greater than about 70%, greater than about 80%, greater than about 90% or greater than about 95%.
  • microcapsules are used to encapsulate flaxseed oil so that the flaxseed oil can be incorporated into a food product while being protected from oxidation or degradation, to hide the taste of the flaxseed oil, and/or to render the flaxseed oil miscible in the food product.
  • the microcapsules containing the flaxseed oil are incorporated into a dairy product, for example, milk, cheese, yogurt, sour cream, ice cream or the like.
  • the microcapsules containing the flaxseed oil are incorporated into a dry food product, for example a cereal or granola bar.
  • microcapsules are used to encapsulate an oil rich in omega-3 fatty acids, e.g. fish oil, so that the oil can be incorporated into a food product while being protected from oxidation or degradation, to hide the taste of the oil, and/or to render the oil miscible in the food product.
  • the microcapsules containing the oil are incorporated into a dairy product, for example, milk, cheese, yogurt, sour cream, ice cream or the like.
  • the microcapsules containing the oil are incorporated into a dry food product, for example a cereal or granola bar.
  • the microcapsules produced by the methods described above have a final moisture content of between about 2% and about 4%, or any value therebetween, e.g. 2.2%, 2.4%, 2.6%, 2.8%, 3.0%, 3.2%, 3.4%, 3.6% or 3.8%.
  • the microcapsules have a water activity of between about 0.05 and about 0.2 or any value therebetween, e.g. 0.06, 0.07, 0.08, 0.09, 0.10, 0.11, 0.12, 0.13, 0.14, 0.15, 0.16, 0.17, 0.18 or 0.19.
  • the microcapsules have L (lightness), a (redness), and b (yellowness) tristimulus colour values including L values ranging from about 87 to about 93 or any value therebetween, e.g. 88, 89, 90, 91, or 92; a values ranging from about -0.5 to about 0.5 or any value there between, e.g. -0.4, -0.3, -0.2, -0.1, 0, 0.1, 0.2, 0.3 or 0.4; and b values ranging from about 8 to about 21 or any value therebetween, e.g. 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19 or 20.
  • the microcapsules have L (lightness), a (redness), and b (yellowness) tristimulus colour values including L values ranging from about 77 to 89 or any value therebetween, e.g. 78, 79, 80, 81, 82, 83, 84, 85, 86, 87 or 88; a values ranging from about 1.4 to about 2.9 or any value therebetween, e.g. 1.5, 1.6, 1.7, 1.8, 1.9, 2.0, 2.1, 2.2, 2.3, 2.4, 2.5, 2.6, 2.7 or 2.8; and b values ranging from about 11 to about 21 or any value therebetween, e.g. 12, 13, 14, 15, 16, 17, 18, 19 or 20.
  • the surface oil content of the microcapsules ranges from about 0.5% to about 20% or any value therebetween, e.g. 1%, 2%, 3%, 4%, 5%, 6%, 8%, 10%, 12%, 14%, 16% or 18%.
  • the encapsulation efficiency (or ratio of the total oil minus the surface oil to the total oil in the microcapsules) is in the range of about 45% to about 95% or any value therebetween, e.g. 50%, 55%, 60%, 65%, 70%, 75%, 80%, 82%, 84%, 86%, 88%, 90%, 91%, 92%, 93% or 94%.
  • the volume-weighted mean droplet diameter range of the emulsion solution is between about 2 and about 5 ⁇ or any value therebetween, e.g. 2.2, 2.4, 2.6, 2.8, 3.0, 3.2, 3.4, 3.6, 3.8, 4.0, 4.2, 4.4, 4.6 or 4.8 ⁇ .
  • the volume- weighted mean droplet diameter range of the microcapsules when redispersed as an emulsion in aqueous solution is between about 1.8 and 12 ⁇ or any value therebetween, e.g. 2, 3, 4, 5, 6, 7, 8, 9, 10 or 11 ⁇ .
  • the volume- weighted mean oil droplet diameter range of the emulsion solution is between about 16 and 24 ⁇ or any value therebetween, e.g. 17, 18, 19, 20, 21, 22 or 23 ⁇ .
  • the volume- weighted mean droplet diameter range of the microcapsules when redispersed as an emulsion in aqueous solution is between about 10 and about 30 ⁇ or any value therebetween, e.g. 12, 14, 16, 18, 20, 22, 24, 26 or 28 ⁇ .
  • the peroxide value of the microcapsules is between about 5 and about 7 meq active 0 2 /kg or any value therebetween, e.g. 5.2, 5.4, 5.6, 5.8, 6.0, 6.2, 6.4, 6.6 or 6.8 meq active 0 2 /kg. In some embodiments, the peroxide value of the microcapsules is between about 5 and about 8 meq active 0 2 /kg or any value therebetween over a 25-day storage period.
  • the production of secondary oxidation products of the microcapsules measured using a 2-thiobarbituric acid reactive substances (TBARS) test is between about 1.5 and about 2.5 MDA eq nmol/mg or any value therebetween, e.g. 1.6, 1.7, 1.8, 1.9, 2.0, 2.1, 2.2, 2.3 or 2.4 MDA eq nmol/mg.
  • the production of secondary oxidation products as measured using a TBARS test over a 25- day storage period is within the aforementioned range, i.e. between about 1.5 and about 2.5 MDA eq nmol/mg or any value therebetween.
  • the material to be encapsulated can be released from the microcapsules by the pH or ionic strength of a solution in which the microcapsules are dispersed.
  • the microcapsules release between about 5% and about 6% of the encapsulated flaxseed oil after one hour at pH 3.0; between about 2.5% and about 5% of the encapsulated flaxseed oil after one hour at pH 5.0; between about 6% and 10% of the encapsulated flaxseed oil after one hour at pH 7.0; and between about 6% and 10% of the encapsulated flaxseed oil after one hour at pH 9.0.
  • the microcapsules release between about 3% and about 6% of the encapsulated flaxseed oil after one hour at 0 mM NaCl; between about 4% and 8% of the encapsulated flaxseed oil after one hour at 50 mM NaCl; between about 6% and 9% of the encapsulated flaxseed oil after one hour at 100 mM NaCl; between about 6% and 10% of the encapsulated flaxseed oil after one hour at 150 mM NaCl; and between about 8% and 11% of the encapsulated flaxseed oil after one hour at 200 mM NaCl.
  • the microcapsules release between about 35% and 45% of the encapsulated flaxseed oil after two hours in simulated gastric fluid, and release between about 80% and 95% of the encapsulated flaxseed oil after two hours in simulated gastric fluid followed by three hours in simulated intestinal fluid.
  • Chickpea (CDC Frontier, Kabuli) and lentil (CDC Grandora) seeds were provided by the Crop Development Centre at the University of Saskatchewan (Saskatoon, SK, Canada).
  • Maltodextrin samples (DE 9, Dry MDTM 01918 and DE 18, Dry MDTM 01909- Z) were donated by Cargill Inc. (Cargill Texturizing Solutions, Cedar Rapids, IA, USA).
  • Flaxseed oil was donated by Bioriginal Food & Science Corp. (Saskatoon, SK, Canada). All chemicals used were of reagent grade and purchased from Sigma-Aldrich (Oakville, ON, Canada). The water used in this research was produced from a Millipore Milli-QTM water system (Millipore Corp., Milford, MA, USA).
  • maltodextrin-DE 9 The chemical composition of maltodextrin-DE 9 was determined to be: 4.6% moisture, 0.0% protein, 0.0% lipid, 95.0% carbohydrate and 0.4% ash.
  • maltodextrin- DE 18 the results were: 4.7% moisture, 0.0% protein, 0.0% lipid, 95.0% carbohydrate and 0.3% ash.
  • Chickpea protein isolate was prepared according to the method of Papalamprou et al. (2010). In brief, defatted flour (100 g) was mixed with water at a 1:10 ratio (w/v), adjusted to pH 9.0 using 1.0 M NaOH and stirred at 500 rpm for 45 minutes at room temperature (21-23°C). The suspension was then centrifuged at 4,500 x g for 20 minutes at 4°C using a Sorvall RC-6 Plus centrifuge (Thermo Scientific, Asheville, NC, USA) to collect the supernatant.
  • the resulting pellet was re- suspended in water at a ratio of 1:5 (w/v), adjusted to pH 9.0, stirred for an additional 45 minutes, followed by centrifugation (4,500 x g, 20 min, 4°C). Supernatants were pooled and adjusted to pH 4.6 using 0.1 M HC1 to precipitate the protein. The protein was recovered by centrifugation as above, collected and stored at -30°C until freeze-drying which was performed using a Labconco FreeZone 6 freeze drier (Labconco Corp., Kansas City, MO, USA) to yield a free flowing powder. Proximate analysis of CPI showed a chemical composition of, 85.40% protein, 6.52% moisture, 3.05% ash, 4.11% carbohydrate and 0.92% lipid.
  • Lentil protein isolate was produced employing the combined methods of Bamdad, Goli, & Kadivar (2006) and Lee, Htoon, & Paterson (2007).
  • Defatted flour 100 g was mixed with water at a 1:10 ratio (w/v), adjusted to pH 9.5 with 1.0 M NaOH, and stirred at 500 rpm for 1 hour at room temperature. The mixture was kept static at 4°C overnight to allow for non-protein sedimentation. After centrifugation at 1,600 x g for 30 minutes at 4°C, the supernatant was collected, and pH was adjusted to 4.5 with 0.1 M HC1.
  • the precipitated protein was collected by centrifugation (1,600 x g, 30 min, 4°C) and stored at -30°C until freeze-drying.
  • Proximate analysis of LPI showed a chemical composition of, 81.90% protein, 5.04% moisture, 3.63% ash, 9.00% carbohydrate and 0.43% lipid.
  • protein solutions were prepared by dispersing the isolates (corrected on a weight basis for protein content) in water followed by adjustment to pH 3.0 or 7.0 with either 0.1 M NaOH or 0.1 M HC1. The resulting mixtures were stirred at 500 rpm overnight at 4°C to ensure complete dispersion.
  • Maltodextrin solutions were prepared by dispersing either DE 9 or 18 in water followed by stirring at 300 rpm overnight at 4°C. Prior to sample homogenization, the pH of the protein solutions was re-adjusted to 3.0 or 7.0 as described above.
  • protein solutions were prepared by dispersing the isolates (corrected on a weight basis for protein content) in water followed by adjustment to pH 3.0 with 0.1 M HCl. The resulting mixtures were stirred at 500 rpm overnight at 4°C to ensure complete dispersion. Maltodextrin solutions were prepared by dispersing the samples in water followed by stirring at 300 rpm overnight at 4°C. Prior to the homogenization, pH of the protein solutions was re-adjusted to 3.0.
  • Oil-in-water emulsions were prepared by homogenizing varying amounts of protein solutions, maltodextrin solution and flaxseed oil (Table 2) in a 500 mL container by using Omni Macro Homogenizer (Omni International, Marietta, GA, USA) with a 20 mm saw tooth generating probe at speed 4 (-7,200 rpm) for 10 minutes with a sample volume of approximately 400 mL. Results from the corresponding formulations will be denoted by their oil content in the final powder (10, 15 and 20%) for discussion purposes. Table 2. Formulations of CPI- and LPI- stabilized emulsions prior to and following spray drying.
  • Droplet size distributions of initial and reconstituted emulsions were measured using a Mastersizer 2000 laser light scattering instrument (Malvern Instruments Ltd., Worcestershire, United Kingdom) equipped with a Hydro 2000S sample handling unit (containing water). Emulsion samples were taken from the bottom of the tube immediately after homogenization for analysis. This sample was stirred continuously within the sample cell to ensure homogeneity at room temperature. Obscuration in all the measurements was kept at -14% by water addition. Droplet size distributions were calculated by the instrument according to the Mie Theory which uses the refractive index difference between the droplets and the dispersing medium to predict the intensity of the scattered light.
  • n t is the number of droplets of diameter ( ⁇ 3 ⁇ 4) (McClements, 2005).
  • Freeze-dried or spray-dried microcapsule samples of 0.5 g were dispersed in 4 mL of water and stirred at 500 rpm for 5 minutes. Samples were withdrawn for particle size distribution with measurements performed as described above. 1.7 Freeze-Dr ing
  • the emulsion samples were spray-dried by a mini spray drier B-290 (Biichi Labortechnik AG, Flawil, Switzerland) with an atomizer nozzle of 700 ⁇ diameter.
  • the dryer had an evaporation rate of 1 L/h and a chamber with diameter of 70 cm.
  • the inlet air temperature was adjusted to 180°C, and the outlet temperature was kept at 90 + 3°C by controlling the flow rate.
  • the emulsions were gently stirred using a magnetic stirrer while fed into the spray dryer.
  • the spray-dried microcapsules were collected in the cyclone collection vessel.
  • microcapsules The moisture content of microcapsules was determined gravimetrically, following drying in a forced-air oven at 105°C for -12 h.
  • Microcapsule water activity was determined using an AquaLab CX-2 water activity meter (Decagon Devices, Inc., Pullman, WA, USA).
  • tristimulus colour values of microcapsules were measured using a Hunter colourimeter (ColorFlex EZ 45/0, Hunter Associates Laboratory, Inc., Reston, VA, USA), which was standardized using a white reference tile. The results were expresses as L (lightness), a (redness), and b (yellowness) tristimulus values.
  • Microcapsule surface oil was determined according to the method of Liu et al. (2010). Briefly, 1 g of microcapsules (freeze-dried) or 2 g of microcapsules (spray-dried) was dispersed in 30 mL of hexane followed by vigorous shaking for 30 seconds. The solvent was filtered (Whatman Gr. 1 paper) into a 40 mL beaker, and the beaker plus solvent was placed in a fume hood overnight to afford solvent evaporation. Microcapsule surface oil was then determined gravimetrically, after heating the beaker at 105°C for 30 minutes to remove any residual solvent.
  • Total oil content of the microcapsules was determined using the method described by Klinkesorn, Sophanodora, Chinachoti, Decker & McClements (2006) with some modifications. Briefly, 4 mL (freeze-dried) or 8 mL (spray-dried) of water was added to 1 g (freeze-dried) or 2 g (spray-dried) of microcapsules followed by mixing at 300 rpm for 2 min.
  • the resulting solution was then mixed with 25 mL (freeze-dried) or 40 mL (spray- dried) hexane/isopropanol (3:1 v/v), stirred at 300 rpm for 15 min and centrifuged at 1500 x g for 2 min. The clear organic phase was collected and the aqueous phase was re- extracted with the aforementioned solvent mixture. The organic phases were pooled and filtered through anhydrous Na 2 S0 4 , and the solvent was allowed to evaporate overnight in a fume hood. Total oil content was determined gravimetrically, after heating at 105°C for 30 min.
  • Microcapsule samples were mounted onto aluminum stubs with double-sided tape and gold coated with a sputter coater. The coated samples were then viewed with a Philips SEM 505 (Eindhoven, The Netherlands) operating at an accelerating voltage of 27 kV with 6x and lOOOx magnification.
  • Oxidative stability of free (i.e. control) and encapsulated flaxseed oil was characterized during storage at room temperature over a 25 day period employing both the peroxide value and 2-thiobarbituric acid reactive substances tests.
  • Microcapsules (3-4 g/bottle freeze-dried or 5 g/bottle spray-dried) or free oil (-2 mL freeze-dried or ⁇ 3 mL spray-dried) were stored in individually sealed nitrogen-flushed 10 mL amber glass bottles for storage stability studies. Oxidative testing was carried out every 5 days over the 25 day testing period, using a new set of unopened samples (i.e. an unopened bottle of microcapsules and oil). Flaxseed oil extraction from the microcapsules followed the same procedure as that outlined previously for total oil determination, except the extraction solvent was dried under a stream of nitrogen.
  • PV (S - B) x Nx l000 / W [eq. 3] where S is the volume of Na 2 S 2 03 added to the sample, B is the volume of Na 2 S 2 03 of the blank, N is the normality of Na 2 S 2 03 solution, and W is the sample weight (g) (Pegg, 2005).
  • a standard curve was prepared using malondialdehyde (MDA) (1.25-50 ⁇ ) under the same experimental conditions. Samples and standards were then heated at 95°C for 1 h. After cooling in cold water, 0.9 mL of n-butanol/pyridine (15:1, v/v) was added, followed by vigorous shaking for 30 s. Samples and standards were centrifuged at 4000 x g for 10 min, and the upper organic layer was transferred to a 1.5 mL cuvette and the absorbance at 532 nm was measured against a butanol blank. TBA values were expressed as mg MDA eq/mg oil, which equates to the MDA content (nmol)/sample oil weight (mg) (modified from Pegg, 2005 and Akhlaghi & Bandy, 2010).
  • microcapsule samples of 1 g (freeze-dried) or 5 g (spray-dried) were individually dispersed in 10 mL (freeze-dried) or 50 mL (spray-dried) aqueous NaCl solutions (0, 50, 100, 150 and 200 mM) that were pH adjusted (0.1 M HCl or NaOH) to produce values of 3.0, 5.0, 7.0 or 9.0 followed by stirring at 500 rpm for 1 h.
  • the amount of released oil was determined by gravimetric analysis after two 30 mL hexane extractions.
  • SGF Simulated gastric fluid
  • SIF Simulated intestinal fluid
  • a 2 g (freeze-dried) or 5 g (spray-dried) microcapsule sample was mixed with 20 mL or 50 mL of SGF, respectively, and incubated for 2 h at 37°C and 100 rpm in a water bath. Released oil was extracted using hexane and then determined gravimetrically.
  • a 2 g (freeze-dried) or 5 g (spray-dried) microcapsule sample was mixed with 20 mL or 50 mL of SGF, respectively, and incubated under the same conditions for 2 h.
  • Moisture content (%) of freeze-dried CPI- and LPI-based microcapsules produced at pH 3.0. Data represent the mean + one standard deviation (n 3).
  • the L (lightness), a (redness), and b (yellowness) tristimulus colour values of freeze dried microcapsules containing flaxseed oil produced at pH 3.0 are presented in Table 5.
  • Microcapsules containing CPI were slightly yellow in colour, which was illustrated by L values ranging from 87.3 to 90.6, a values from -0.5 to 0.3, and b values from 11.2 to 20.3.
  • microcapsules containing LPI were beige in colour with L values ranging from 77.9 to 84.4, a values from 2.1 to 2.9, and b values from 14.1 to 20.1.
  • Surface oil represents the portion of oil present on the surface of the microcapsule (Bao, Hu, Zhang, Xu, Zhang & Huang, 2011). Minimizing the amount of surface oil is important in lipid microencapsulation as this material can potentially oxidize at more rapid rates than the encapsulated oil, causing rancidity and reducing the shelf life of the finished product (Pegg & Shahidi, 2007).
  • the effect of emulsion formulation on surface oil content is presented in Figure 1. It was noted that the surface oil content of the microcapsules produced at pH 3.0 ranged from 0.7-19.8% depending on the formulation.
  • oil concentration p ⁇ 0.001
  • maltodextrin type p ⁇ 0.001
  • interactions between protein source x maltodextrin type p ⁇ 0.05
  • protein source x oil concentration p ⁇ 0.001
  • maltodextrin type x oil concentration p ⁇ 0.001
  • surface oil in the microcapsules increased from 1.0 to 16.9% as the oil concentration in the initial emulsions increased from 5.3 to 21.1%.
  • maltodextrin two types were used as a secondary wall material (i.e., filler) to improve microcapsule drying properties (Kagami et al., 2003).
  • Maltodextrins are widely used as wall materials for capsule formation as they exhibit good solubility and low viscosities at high solids contents (Gharsallaoui, Roudaut, Chambin, Voilley, & Saurel, 2007).
  • microcapsules prepared with maltodextrin-DE 9 had lower surface oil contents (6.5%) when compared to microcapsules prepared with maltodextrin-DE 18 (8.3%).
  • Maltodextrin-DE 18 is a more hydrolyzed starch product with a higher concentration of lower molecular weight glucose polymers, which are responsible for its higher water solubility compared to maltodextrin- DE 9. Without being bound by theory, it is believed that the lower surface oil content observed in microcapsules prepared with DE 9 is most likely due to its higher hydrophobicity when compared to DE 18 due to the presence of higher molecular weight glucose polymers in this material.
  • the volume-weighted mean droplet diameter range ( ⁇ i 4,3 ) of flaxseed oil-in-water emulsions stabilized by CPI and LPI were 2.4-4.8 ⁇ and 2.7-4.5 ⁇ , respectively, depending on the formulation.
  • An analysis of variance revealed that protein source (p ⁇ 0.01), maltodextrin-type (p ⁇ 0.001), flaxseed oil concentration (p ⁇ 0.001), the interactions between protein source x maltodextrin-type (p ⁇ 0.05), protein source x oil concentration (p ⁇ 0.001) and maltodextrin-type x oil concentration (p ⁇ 0.01) were all significant.
  • the ⁇ i 4 3 values increased from -3.1 ⁇ to -4.1 ⁇ .
  • the larger oil droplets observed at oil concentrations >10% could be attributed to the limited availability of protein to cover the oil surface to sufficiently form a dense adsorption layer so as to prevent coalescence.
  • microcapsules containing flaxseed oil that would be suitable for use in food commodities with a more neutral pH such as dairy products.
  • the physicochemical characteristics of microcapsules produced at pH 7.0 are presented in Table 6.
  • Microcapsules produced with CPI at pH 7.0 had lower moisture content and water activity compared to pH 3.0 (p ⁇ 0.05).
  • lower L (lightness) and higher a (redness) and b (yellowness) values were observed in microcapsules produced with CPI at pH 7.0 compared to pH 3.0 (p ⁇ 0.05), resulting in a slightly darker yellowish colour.
  • microcapsules produced with LPI at pH 7.0 maintained their original droplet diameter after water-redispsersion of freeze-dried material while this process resulted in an increase in oil droplet diameter in microcapsules produced with CPI at pH 7.0.
  • Microcapsules produced with LPI at pH 7.0 had similar moisture content (p>0.05) but lower water activity (p ⁇ 0.05) than those produced at pH 3.0.
  • a lower L (lightness) value was found in microcapsules produced with LPI at pH 7.0 compared to pH 3.0 (p ⁇ 0.05).
  • Microcapsules produced with LPI at pH 7.0 and 3.0 had similar surface oil content, encapsulation efficiency and maintained their original droplet diameter after water-redispersion following freeze-drying (p>0.05).
  • FIG. 4 SEM images of freeze-dried CPI- and LPI-based microcapsules containing 10.5% flaxseed oil are shown in Figure 4. All four samples (microcapsules produced at both pH 3.0 and 7.0) had similar surface morphology which were highly porous. A porous microcapsule morphology has also been observed by other research groups for freeze- dried oil-in water emulsions (Anwar & Kunz 2011; Heinzelmann, Franke, Jensen & Haahr 2000). Panel A shows CPI at pH 3.0. Panel B shows LPI at pH 3.0. Panel C shows CPI at pH 7.0. Panel D shows LPI at pH 7.0.
  • a CPI- and LPI-based microcapsule formulation was chosen having 4.0% protein, 35.5% maltodextrin-DE 9, and 10.5% oil.
  • the oxidative stability of free and the CPI- and LPI-based microencapsulated flaxseed oil stored under nitrogen and held at room temperature was monitored over a 25 day period, with sample peroxide value (PV) and TBARS results determined at five-day intervals for all samples (Figure 5).
  • the PV of free flaxseed oil at time zero was 5.88 + 010 meq active 0 2 /kg while that of CPI- or LPI-based microencapsulated flaxseed oil at immediately following freeze drying and extraction (time zero) ranged from 5.76-6.40 meq active 0 2 /kg; with no significant difference observed between protein source (CPI vs. LPI) and pH (3.0 vs. 7.0). Because the PV of time zero microencapsulated flaxseed oil was found to be similar to that of the free oil, the emulsification and encapsulation processes did not negatively impact oil stability.
  • the primary oxidative products (hydroperoxides) measured by the PV test are odourless and colourless but can readily participate in the autoxidation process producing a variety of secondary oxidation products, such as aliphatic aldehydes, alcohols, ketones, cyclic compounds, and hydrocarbons which can have an adverse effect on the sensory attributes of the oil/product (Pegg, 2005).
  • secondary oxidation products were measured using the TBARS test.
  • the TBARS value of CPT and LPI-based microencapsulated flaxseed oil remained unchanged (-1.85 nmol/mg oil at time zero and -2.15 nmol/mg oil at day 25) over the 25 d storage period (p>0.05), with no significant differences observed between protein isolate and pH.
  • the TBARS values for free oil remained unchanged during the first 15 days (2.12-2.51 nmol/mg oil) but increased to 3.22 nmol/mg oil at day 20 and to 3.98 nmol/mg oil at day 25 (p ⁇ 0.05).
  • microencapsulated flaxseed oil release under SGF conditions ranged from 36.6-43.4% with the highest value observed for the CPI capsules prepared at pH 7.0, whereas the lowest value was observed for the LPI capsules prepared at pH 7.0.
  • Microencapsulated flaxseed oil release under the combined SGF-SIF conditions was significantly higher (84.5-92.6%) than that observed for SGF only. Without being bound by theory, this result is most likely explained by the presence of the proteolytic enzyme pepsin in SGF which catalyses protein hydrolysis resulting in a change in capsule structure (e.g. large pore formation) with concomitant oil release.
  • the observed darker colour of the LPI- containing microcapsules may be explained by the hull colour of the lentil proteins used in isolate production (Bamdad et al., 2006).
  • CPI- and LPI-containing microcapsules had similar amounts of surface oil (-1.75% and -1.66%, respectively, p>0.05). However, LPI resulted in significantly higher encapsulation efficiency (-88.0%) compared to CPI (-86.3%, p ⁇ 0.05).
  • CPI- stabilized emulsions had significantly smaller oil droplets (-20.9 ⁇ ) compared to LPI- stabilized emulsions (-23.9 ⁇ , p ⁇ 0.05).
  • effect of oil concentration followed a different trend depending on the protein source.
  • mean oil droplet diameter increased from -16.3 ⁇ to -23.2 ⁇ when the oil concentration increased from 2% to 3-4% in the initial emulsion.
  • mean oil droplet diameter of emulsions containing 3% oil (-21.0 ⁇ ) was significantly lower than that of emulsions containing 2 and 4% oil (-25.3 ⁇ , p ⁇ 0.05).
  • FIG. 7 SEM images of spray-dried microcapsules are shown in Figure 7.
  • Panel A shows CPI and 10% oil.
  • Panel B shows CPI and 15% oil.
  • Panel C shows CPI and 20% oil.
  • Panel D shows LPI and 10% oil.
  • Panel E shows LPI and 15% oil.
  • Panel F shows LPI and 20% oil. Changes in protein source and oil concentration did not affect the morphology of the microcapsules which appeared to be composed of heterogeneous spheres of various sizes. All samples exhibited a rounded external surface and similar surface morphology, which was smooth and free of visible pores or cracks. Surface depression was evident and was also reported in other spray dried particles containing maltodextrin as part of their wall materials (Bae and Lee, 2008; Soottitantawat et al., 2005). 3.3 Oxidative Stability of Encapsulated Flaxseed Oil
  • PV peroxide value
  • TBARS results for free and CPI and LPI encapsulated flaxseed oil maintained at room temperature over a 25 d period are presented in Table 11.
  • the PV of flaxseed oil before microencapsulation was 5.73 + 0.30 meq active 0 2 /kg while that of the microencapsulated oil immediately after spray drying (Day 0) ranged from 6.31-6.80 meq active 0 2 /kg.
  • this increase in PV value for flaxseed oil during the microencapsulation process can be attributed to oxygen contact with oil during the emulsification spray drying processes.
  • the TBARS value of microencapsulated flaxseed oil in both CPI- and LPI-containing microcapsules was between 1.90-2.47 MDA eq/mg oil and did not change over the 25 day storage period (p>0.05, Table 11) showing no significant difference between protein source and oil concentration.
  • TBARS value of bulk oil started to increase from 2.29 to 3.15 nmol MDA eq/mg oil at day 20 and kept increasing to 3.95 MDA eq/mg oil at day 25 (p ⁇ 0.05, Table 11); indicating an increase in secondary oxidative products.
  • Percentage of oil released was found to be the lowest at 0 mM NaCl and increased with increasing ionic strength (p ⁇ 0.05), as it was assumed the addition of NaCl improved solubility of protein isolates. Increased amounts of oil in the microcapsules resulted in increased amounts of released oil (p ⁇ 0.05) regardless of the protein source used in the microcapsules and ionic strength of the release medium.
  • the -40% flaxseed oil release in simulated gastric fluid from the 20% oil microcapsules was significantly higher than the -37% observed for the 10 and 15% oil microcapsules.
  • flaxseed oil released from LPI microcapsules increased from 81.5 to 86.2% as the oil content in the microcapsules increased from 10 to 20%.
  • microcapsules formed using legume proteins can encapsulate an oil or an oil-soluble vitamin that can form an emulsion with water. It can be soundly predicted that such microcapsules can be used to protect the encapsulated oil (for example, by preventing oxidative degradation as demonstrated in Examples 2.4 and 3.3).
  • microcapsules can be used to provide delayed release of the oil in the gastrointestinal tract of an animal based on the results showing that only a small portion of the encapsulated oil is released under pH conditions ranging from 3.0 to 9.0 and an ionic strength ranging from 0 to 200 mM NaCl, while a significant portion of the encapsulated oil is released under simulated gastric and intestinal conditions (Examples 2.5 and 3.4).
  • it can be soundly predicted that such microcapsules are suitable for addition to a food product, including based on results showing a moisture content and water activity within the maximum moisture specification for dried powders in the food industry (Examples 2.1 and 3.1).
  • microcapsules are suitable for addition to a food product having a relatively neutral pH, including based on results showing that only a small portion of the encapsulated oil is released under pH conditions ranging from 3.0 to 9.0 (Examples 2.5 and 3.4).

Landscapes

  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Polymers & Plastics (AREA)
  • Food Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Nutrition Science (AREA)
  • Health & Medical Sciences (AREA)
  • Biochemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Proteomics, Peptides & Aminoacids (AREA)
  • Mycology (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • General Preparation And Processing Of Foods (AREA)
  • Manufacturing Of Micro-Capsules (AREA)

Abstract

L'invention concerne des microcapsules ayant un cœur comprenant un matériau à encapsuler et une enveloppe comprenant une protéine de légume et un glucide de faible poids moléculaire. L'invention concerne des procédés de production des microcapsules.
PCT/IB2013/059458 2012-10-22 2013-10-18 Microencapsulation au moyen de protéines de légume Ceased WO2014064591A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US201261717021P 2012-10-22 2012-10-22
US61/717,021 2012-10-22

Publications (1)

Publication Number Publication Date
WO2014064591A1 true WO2014064591A1 (fr) 2014-05-01

Family

ID=50544101

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/IB2013/059458 Ceased WO2014064591A1 (fr) 2012-10-22 2013-10-18 Microencapsulation au moyen de protéines de légume

Country Status (1)

Country Link
WO (1) WO2014064591A1 (fr)

Cited By (21)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104313005A (zh) * 2014-10-22 2015-01-28 江苏省农业科学院 一种高稳定性乳酸菌微胶囊及其制备方法与应用
CN105166908A (zh) * 2015-10-10 2015-12-23 付强 一种富含ω-3脂肪酸的微囊粉及其制备方法
CN107048421A (zh) * 2017-03-28 2017-08-18 常州大学 一种抗氧化微胶囊壁材的制备方法
WO2017144435A1 (fr) * 2016-02-26 2017-08-31 Dsm Ip Assets B.V. Nouveau système d'enrobage (ii)
CN107484985A (zh) * 2016-06-12 2017-12-19 华中农业大学 一种自乳化鱼油微胶囊及其生产工艺
CN109588495A (zh) * 2018-11-20 2019-04-09 阜阳九珍食品有限公司 一种使用微胶囊包埋技术制备水溶性红油调料粉的方法
CN111955735A (zh) * 2020-07-30 2020-11-20 中国农业大学 一种植物甾醇微胶囊的制备方法
US10904871B2 (en) * 2017-11-29 2021-01-26 Qualcomm Incorporated Aggregation level specific PDCCH modification
CN112450284A (zh) * 2020-11-27 2021-03-09 江西恒顶食品有限公司 一种亚麻籽油脂肪粉的制备方法
US11102998B1 (en) 2017-08-25 2021-08-31 The Hershey Company Binders and methods of making and using the same
CN113397175A (zh) * 2021-06-30 2021-09-17 中国科学院烟台海岸带研究所 一种刺参低聚肽交联微胶囊及其制备方法和应用
CN114982951A (zh) * 2022-06-29 2022-09-02 重庆康菌泰生物科技股份有限公司 一种天然银杏酵素的制备方法
CN115023148A (zh) * 2020-01-24 2022-09-06 国际香料和香精公司 用植物蛋白质进行微包封
WO2022221710A1 (fr) 2021-04-16 2022-10-20 International Flavors & Fragrances Inc. Encapsulations d'hydrogel et leurs procédés de fabrication
CN115226765A (zh) * 2022-01-26 2022-10-25 四川农业大学 一种酶敏感复合膜的制备方法及其应用
CN115279484A (zh) * 2020-03-27 2022-11-01 弗门尼舍有限公司 凝聚层核-壳微胶囊
WO2023239944A3 (fr) * 2022-06-10 2024-01-18 Phyto Tech Corp. Microcapsules biodégradables chargées de parfum et/ou d'arôme
CN118973411A (zh) * 2022-03-31 2024-11-15 喷雾系统公司 静电喷雾干燥的活性化合物粉末及其生产方法
CN119255717A (zh) * 2022-01-03 2025-01-03 喷雾系统公司 静电喷雾干燥的油粉末及其生产方法
EP4391830A4 (fr) * 2021-08-25 2025-06-25 Technion Research & Development Foundation Limited Microparticules constituées d'extraits de protéines végétales et leurs utilisations en tant que supports cellulaires pour la préparation de produits alimentaires
WO2025242779A1 (fr) 2024-05-23 2025-11-27 Nucaps Nanotechnology, S.L. Particules pour l'incorporation de substances actives, capsules et leur procédé d'obtention

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6596337B1 (en) * 1998-02-02 2003-07-22 Rhodia Chimie Food composition in the form of a dry emulsion, preparation method and use thereof
WO2009070010A1 (fr) * 2007-11-29 2009-06-04 Nizo Food Research B.V. Capsules d'huile à base de protéine
EP2457451A1 (fr) * 2007-08-28 2012-05-30 PepsiCo, Inc. Administration et libération contrôlée de nutriment lipophile encapsulé

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6596337B1 (en) * 1998-02-02 2003-07-22 Rhodia Chimie Food composition in the form of a dry emulsion, preparation method and use thereof
EP2457451A1 (fr) * 2007-08-28 2012-05-30 PepsiCo, Inc. Administration et libération contrôlée de nutriment lipophile encapsulé
WO2009070010A1 (fr) * 2007-11-29 2009-06-04 Nizo Food Research B.V. Capsules d'huile à base de protéine

Cited By (27)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104313005A (zh) * 2014-10-22 2015-01-28 江苏省农业科学院 一种高稳定性乳酸菌微胶囊及其制备方法与应用
CN105166908A (zh) * 2015-10-10 2015-12-23 付强 一种富含ω-3脂肪酸的微囊粉及其制备方法
WO2017144435A1 (fr) * 2016-02-26 2017-08-31 Dsm Ip Assets B.V. Nouveau système d'enrobage (ii)
CN108697120A (zh) * 2016-02-26 2018-10-23 帝斯曼知识产权资产管理有限公司 新颖的包衣体系（ii）
CN107484985A (zh) * 2016-06-12 2017-12-19 华中农业大学 一种自乳化鱼油微胶囊及其生产工艺
CN107484985B (zh) * 2016-06-12 2020-01-10 华中农业大学 一种自乳化鱼油微胶囊及其生产工艺
CN107048421A (zh) * 2017-03-28 2017-08-18 常州大学 一种抗氧化微胶囊壁材的制备方法
US11102998B1 (en) 2017-08-25 2021-08-31 The Hershey Company Binders and methods of making and using the same
US10904871B2 (en) * 2017-11-29 2021-01-26 Qualcomm Incorporated Aggregation level specific PDCCH modification
CN109588495A (zh) * 2018-11-20 2019-04-09 阜阳九珍食品有限公司 一种使用微胶囊包埋技术制备水溶性红油调料粉的方法
CN115023148A (zh) * 2020-01-24 2022-09-06 国际香料和香精公司 用植物蛋白质进行微包封
CN115279484A (zh) * 2020-03-27 2022-11-01 弗门尼舍有限公司 凝聚层核-壳微胶囊
CN111955735A (zh) * 2020-07-30 2020-11-20 中国农业大学 一种植物甾醇微胶囊的制备方法
CN111955735B (zh) * 2020-07-30 2022-04-29 中国农业大学 一种植物甾醇微胶囊的制备方法
CN112450284A (zh) * 2020-11-27 2021-03-09 江西恒顶食品有限公司 一种亚麻籽油脂肪粉的制备方法
CN112450284B (zh) * 2020-11-27 2023-05-12 江西恒顶食品有限公司 一种亚麻籽油脂肪粉的制备方法
WO2022221710A1 (fr) 2021-04-16 2022-10-20 International Flavors & Fragrances Inc. Encapsulations d'hydrogel et leurs procédés de fabrication
US20240180220A1 (en) * 2021-04-16 2024-06-06 International Flavors & Fragrances Inc. Hydrogel encapsulations and methods of making the same
CN113397175A (zh) * 2021-06-30 2021-09-17 中国科学院烟台海岸带研究所 一种刺参低聚肽交联微胶囊及其制备方法和应用
CN113397175B (zh) * 2021-06-30 2022-12-23 中国科学院烟台海岸带研究所 一种刺参低聚肽交联微胶囊及其制备方法和应用
EP4391830A4 (fr) * 2021-08-25 2025-06-25 Technion Research & Development Foundation Limited Microparticules constituées d'extraits de protéines végétales et leurs utilisations en tant que supports cellulaires pour la préparation de produits alimentaires
CN119255717A (zh) * 2022-01-03 2025-01-03 喷雾系统公司 静电喷雾干燥的油粉末及其生产方法
CN115226765A (zh) * 2022-01-26 2022-10-25 四川农业大学 一种酶敏感复合膜的制备方法及其应用
CN118973411A (zh) * 2022-03-31 2024-11-15 喷雾系统公司 静电喷雾干燥的活性化合物粉末及其生产方法
WO2023239944A3 (fr) * 2022-06-10 2024-01-18 Phyto Tech Corp. Microcapsules biodégradables chargées de parfum et/ou d'arôme
CN114982951A (zh) * 2022-06-29 2022-09-02 重庆康菌泰生物科技股份有限公司 一种天然银杏酵素的制备方法
WO2025242779A1 (fr) 2024-05-23 2025-11-27 Nucaps Nanotechnology, S.L. Particules pour l'incorporation de substances actives, capsules et leur procédé d'obtention

Similar Documents

Publication Publication Date Title
WO2014064591A1 (fr) Microencapsulation au moyen de protéines de légume
Karaca et al. Microcapsule production employing chickpea or lentil protein isolates and maltodextrin: Physicochemical properties and oxidative protection of encapsulated flaxseed oil
Can Karaca et al. Encapsulation of flaxseed oil using a benchtop spray dryer for legume protein–maltodextrin microcapsule preparation
Fraj et al. Encapsulation and release of vitamin C in double W/O/W emulsions followed by complex coacervation in gelatin-sodium caseinate system
Burgos-Díaz et al. Multilayer emulsions stabilized by vegetable proteins and polysaccharides
CN106659230B (zh) 疏水性生物活性化合物的包封
González et al. Study of the preparation process and variation of wall components in chia (Salvia hispanica L.) oil microencapsulation
Barrow et al. Spray drying and encapsulation of omega-3 oils
Wilson et al. Microencapsulation of vitamins
Chang et al. Microencapsulation of canola oil by lentil protein isolate-based wall materials
Devi et al. Effect of gelatin and acacia gum on anthocyanin coacervated microcapsules using double emulsion and its characterization
Wang et al. Coacervation technique as an encapsulation and delivery tool for hydrophobic biofunctional compounds
Chuacharoen et al. The potential of zein nanoparticles to protect entrapped β-carotene in the presence of milk under simulated gastrointestinal (GI) conditions
Pavani et al. Novel encapsulation approaches for phytosterols and their importance in food products: A review
Neekhra et al. Innovative approaches for microencapsulating bioactive compounds and probiotics: An updated review
Abbasi et al. A critical review on the bioavailability promotion of the food bioactive compounds: nano lipid carriers perspective
Farrag et al. Research Article Microencapsulation of Grape Phenolic Compounds Using Whey Proteins as a Carrier Vehicle
Jokar et al. Microencapsulation of fish oil rich in EPA and DHA using mixture of Arabic gum and Persian gum through spray‐drying technique
Quek et al. Microencapsulation of food ingredients for functional foods
Rani et al. Encapsulation methods in the food industry: Mechanisms and applications
Altuntas et al. Enhanced oxidative stability and bioaccessibility of sour cherry kernel byproducts encapsulated by complex coacervates with different wall matrixes by spray-and freeze-drying
Kim et al. Development of turmeric extract nanoemulsions and their incorporation into canned ham
Özbek et al. Influence of wall material composition on microencapsulation efficiency of cold pressed pumpkin seed oil by Freeze-Drying
Rahmani-Manglano et al. The role of antioxidants and encapsulation processes in omega-3 stabilization
Pittia et al. Conventional product formation

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 13848353

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 13848353

Country of ref document: EP

Kind code of ref document: A1