WO2024114679A1 - Microcapsule for intestinal-targeted release and preparation method therefor, and food composition - Google Patents

Microcapsule for intestinal-targeted release and preparation method therefor, and food composition Download PDF

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Publication number
WO2024114679A1
WO2024114679A1 PCT/CN2023/134990 CN2023134990W WO2024114679A1 WO 2024114679 A1 WO2024114679 A1 WO 2024114679A1 CN 2023134990 W CN2023134990 W CN 2023134990W WO 2024114679 A1 WO2024114679 A1 WO 2024114679A1
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Prior art keywords
layer
wrapping
microcapsules
intestinal
gelatin
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PCT/CN2023/134990
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French (fr)
Chinese (zh)
Inventor
杨帆
查琳琳
巴根纳
侯廷帅
谭圣杰
孙倩
孙彦文
Original Assignee
内蒙古伊利实业集团股份有限公司
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Publication of WO2024114679A1 publication Critical patent/WO2024114679A1/en

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    • 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; MAKING 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
    • 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; MAKING 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
    • A23F—COFFEE; TEA; THEIR SUBSTITUTES; MANUFACTURE, PREPARATION, OR INFUSION THEREOF
    • A23F3/00—Tea; Tea substitutes; Preparations thereof
    • A23F3/06—Treating tea before extraction; Preparations produced thereby
    • A23F3/14—Tea preparations, e.g. using additives
    • 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
    • A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
    • A23L27/60—Salad dressings; Mayonnaise; Ketchup
    • 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
    • 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
    • A23L29/10—Foods or foodstuffs containing additives; Preparation or treatment thereof containing emulsifiers
    • 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
    • A23L29/30—Foods or foodstuffs containing additives; Preparation or treatment thereof containing carbohydrate syrups; containing sugars; containing sugar alcohols, e.g. xylitol; containing starch hydrolysates, e.g. dextrin
    • 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
    • A23L33/10—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
    • 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
    • A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/135—Bacteria or derivatives thereof, e.g. probiotics
    • 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
    • A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/15—Vitamins
    • 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
    • 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
    • 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
    • A23P20/00—Coating of foodstuffs; Coatings therefor; Making laminated, multi-layered, stuffed or hollow foodstuffs
    • A23P20/10—Coating with edible coatings, e.g. with oils or fats
    • A23P20/12—Apparatus or processes for applying powders or particles to foodstuffs, e.g. for breading; Such apparatus combined with means for pre-moistening or battering
    • 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
    • A23P20/00—Coating of foodstuffs; Coatings therefor; Making laminated, multi-layered, stuffed or hollow foodstuffs
    • A23P20/10—Coating with edible coatings, e.g. with oils or fats
    • A23P20/15—Apparatus or processes for coating with liquid or semi-liquid products
    • 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
    • A23P20/00—Coating of foodstuffs; Coatings therefor; Making laminated, multi-layered, stuffed or hollow foodstuffs
    • A23P20/20—Making of laminated, multi-layered, stuffed or hollow foodstuffs, e.g. by wrapping in preformed edible dough sheets or in edible food containers
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12N—MICROORGANISMS OR ENZYMES; COMPOSITIONS THEREOF; PROPAGATING, PRESERVING, OR MAINTAINING MICROORGANISMS; MUTATION OR GENETIC ENGINEERING; CULTURE MEDIA
    • C12N11/00—Carrier-bound or immobilised enzymes; Carrier-bound or immobilised microbial cells; Preparation thereof
    • C12N11/02—Enzymes or microbial cells immobilised on or in an organic carrier
    • C12N11/04—Enzymes or microbial cells immobilised on or in an organic carrier entrapped within the carrier, e.g. gel or hollow fibres

Definitions

  • the present invention relates to the field of food technology, and in particular to an intestinal directional release microcapsule, a preparation method thereof and a food composition.
  • Microencapsulation technology uses an embedding material to encapsulate the target core material (solid, liquid or even gas) to form a microcapsule with a diameter ranging from 1 to 5000 ⁇ m and a semi-permeable or sealed capsule membrane.
  • Probiotics can produce a variety of active substances and play an important role in regulating the balance of intestinal microecology and preventing and treating certain diseases. However, most probiotics are not acid-resistant. After passing through the gastric juice and bile salt environment at the upper end of the digestive tract, the number of live bacteria drops significantly, which will affect the efficacy of the product. Making probiotics into microcapsules is currently one of the most effective and promising methods to solve the acid resistance of probiotics. Microcapsules can provide an effective physical barrier for probiotics, ensuring that a certain number of probiotics survive in the digestive tract and are released in a targeted manner in the small intestine.
  • Chinese patent CN115039886A discloses a bifidobacterium microcapsule, which uses porous starch as a protective agent, loads bifidobacteria, and then uses xanthan gum-trehalose-casein-sodium alginate, pectin-sodium alginate and zein alcohol solution for three times of coating to obtain a three-layer coated microcapsule.
  • the microcapsule has good acid and bile salt resistance, it releases live bacteria in the intestine slowly.
  • the technical problem to be solved by the present invention is to provide an intestinal directional release microcapsule, a preparation method thereof and a food composition.
  • the intestinal directional release microcapsule provided by the present invention has good acid resistance, can be directed released in the intestine, and can be completely released within 90 to 120 minutes.
  • the present invention provides an intestinal directional release microcapsule, comprising:
  • the core material comprising an active ingredient
  • first wall material layer wrapping the core material, the first wall material layer comprising gelatin and sodium alginate, wherein the content of the gelatin is at least 20 wt %;
  • a second wrapping layer wrapping the first wall material layer, wherein the second wrapping layer is formed of a powdery substance
  • the intestinal directional release microcapsule provided by the present invention has a three-layer packaging structure, which not only has good acid resistance and can be directed to the intestinal tract, but also can be released within 90 to 120 minutes.
  • the core material includes an active ingredient, which is selected from one or more of probiotics, prebiotics, vitamins and DHA, preferably probiotics.
  • the core material also includes oils and emulsifiers, wherein the oils can be vegetable oils, such as coconut oil, vegetable mixed oils, and palm oil; the emulsifier is selected from polyol fatty acid esters, including propylene glycol fatty acid esters, glycerol fatty acid esters, sugar esters, polyglycerol fatty acid esters, phospholipids, sodium caseinate, etc.
  • the core material may include: 1wt% to 99wt% of oils; 1wt% to 50wt% of active ingredients; and 0 to 20wt% of lubricants.
  • the core material includes 20wt% to 80wt% of oils; 10wt% to 40wt% of active ingredients; and 10 to 20wt% of emulsifiers.
  • the core material includes 20wt% to 80wt% of oils; 10wt% to 20wt% of probiotics; 10wt% to 20wt% of prebiotics and 10 to 20wt% of emulsifiers.
  • the intestinal directional release microcapsule provided by the present invention includes a first wall material layer wrapping the core material, the first wall material layer includes gelatin and sodium alginate, and the content of the gelatin is at least 20wt%.
  • the first wall material layer formed by gelatin and sodium alginate makes the microcapsule wall porosity lower, so that the capsule is released in the intestine within 90 to 120 minutes.
  • the mass ratio of gelatin and sodium alginate is 3 to 10: 0.3 to 5, preferably 4 to 8: 1 to 4.
  • the first wall material layer also includes agar, and the mass ratio of agar, gelatin and sodium alginate is 3 to 15: 3 to 10: 0.3 to 5, more preferably 4 to 10: 4 to 8: 1 to 4.
  • the mass ratio of the core material to the first wall material is 3: 4 to 6, preferably 3: 5.
  • the thickness of the first wall material is 1.5 to 2.5 mm, preferably 2 mm.
  • the first wall material layer also includes a calcified crosslinking agent to solidify and harden the wall material formed by gelatin and sodium alginate to obtain a hard capsule.
  • the calcified crosslinking agent includes but is not limited to calcium chloride or calcium lactate, preferably calcium chloride.
  • the mass ratio of the calcified crosslinking agent to sodium alginate is 1:4 to 6, preferably 1:5.
  • the particle size of the microcapsules wrapped in the first layer of wall material is 0.5 to 15 mm, preferably 1 to 10 mm, and more preferably 3 to 8 mm.
  • the intestinal directional release microcapsules provided by the present invention include a second wrapping layer wrapping the first wall material layer, and the second wrapping layer is formed by a powdery substance.
  • the powdery substance provides a specific flavor for the microcapsules on the one hand, and increases the acid resistance of the microcapsules on the other hand, while not affecting the release of the microcapsules in the intestine.
  • the powdery substance includes flavor substance powder, such as one or more of cheese powder, starch, protein powder and fruit powder; it can also be functional powder, such as dietary fiber, VC, VB, DHA and other nutritional enhancers, and can also be colloidal powder, such as cassava flour.
  • the thickness of the second wrapping layer is 1.5 to 2.5 mm, preferably 2 mm.
  • the mass ratio of the second wrapping layer to the core material is 1:1.5 to 3, preferably 1:2.
  • the intestinal directional release microcapsules provided by the present invention include a third wrapping layer wrapping the second wrapping layer, and the third wrapping layer is formed by a gum-like substance.
  • the gum-like substance gives the microcapsules a special taste on the one hand, and increases the acid resistance of the microcapsules on the other hand, while not affecting the release of the microcapsules in the intestine.
  • the gum-like substance is selected from one or more of konjac gum, carrageenan, sodium alginate, gellan gum, sodium carboxymethyl cellulose, xanthan gum, agar, pectin and gelatin, preferably including at least sodium alginate.
  • the thickness of the third wrapping layer is 2 to 4 mm, preferably 3 mm.
  • the mass ratio of the third wrapping layer to the core material is 1:2 to 5, preferably 1:4.
  • the microcapsule provided by the present invention comprises three layers of wall materials, namely a sodium alginate and gelatin layer, a powder coating layer and a gelatin coating layer.
  • the three-layer structure not only makes the microcapsule acid-resistant and can be released in the intestine, but also has a release time in the intestine of 90 to 120 minutes. More importantly, it can increase the flavor and taste of the microcapsule.
  • the present invention also provides a method for preparing the intestinal directional release microcapsules described in the above technical solution, comprising the following steps:
  • a core material including an active ingredient is encapsulated with a mixture including gelatin and sodium alginate as a first layer of wall material to form a single-layer microcapsule including the core material and the first wall material layer; the content of gelatin in the mixture is at least 20 wt%;
  • the double-layer wrapped microcapsules are wrapped with a glue-like substance to form triple-layer wrapped microcapsules.
  • the present invention first heats and mixes gelatin and sodium alginate as wall materials to form a wall material solution, and then embeds the core material including the active ingredient in the wall material solution to form a microcapsule in which the wall material encapsulates the core material.
  • the selection and dosage of the core material and the wall material are as described above, and the present application will not repeat them here.
  • the embedding of the drop pills can be carried out in a manner well known to those skilled in the art, and the present application will not repeat them here.
  • the microcapsules after the microcapsules with the wall material encapsulating the core material are formed, the microcapsules are placed in a calcified The microcapsules are calcified and cross-linked in a cross-linking agent solution, wherein the cross-linking agent is selected from calcium chloride or calcium lactate.
  • the concentration of the cross-linking agent solution is 1 to 20 wt%, preferably 5 to 15 wt%.
  • the microcapsules are immersed in the cross-linking agent solution for 30 to 90 minutes to solidify the wall material.
  • the obtained single-layer microcapsules are wrapped with a powdery substance for a second layer.
  • the present invention has no particular limitation on the method of wrapping the single-layer microcapsules with a powdery substance for a second layer.
  • the single-layer microcapsules can be mixed with the powdery substance to wrap the powdery substance on the single-layer microcapsules.
  • the powdery substance can be mixed with water to form a suspension, mixed with the single-layer microcapsules, and the powdery substance can be wrapped on the outer layer of the microcapsules, and then dried.
  • the obtained double-layer microcapsules are wrapped with a glue-like substance for a third layer.
  • the present invention has no special restrictions on the method of wrapping the double-layer microcapsules with a glue-like substance for a third layer.
  • the double-layer microcapsules are mixed with a glue-like substance solution, and the glue-like substance is wrapped on the surface of the double-layer microcapsules. After drying, the third layer can be formed.
  • the microcapsules After the microcapsules are prepared, they can also be prepared into a sauce, which includes water, a sweetener and the above-mentioned microcapsules, and the pH value of the sauce is acidic. Specifically, water and a sweetener are first mixed, the pH value of the obtained mixed solution is adjusted to acidic, and the mixture is sterilized after mixing with the above-mentioned microcapsules to obtain a sauce.
  • the sterilization temperature is 65°C to 121°C, preferably 70°C to 115°C, and more preferably 80°C to 100°C; the sterilization time is 4s to 30min, preferably 1min to 25min, and more preferably 5min to 20min.
  • the present invention has no special restrictions on the content of microcapsules in the sauce, which can be 5wt% to 80wt%, preferably 10wt% to 70wt%.
  • the present invention has no special restrictions on the sweetener, and white sugar, fructose, lactose and other sweet ingredients can be used.
  • the microcapsule provided by the present invention comprises three layers of wall materials, namely a sodium alginate and gelatin layer, a powder coating layer and a gelatin coating layer.
  • the three-layer structure not only makes the microcapsule acid-resistant and can be released in the intestine, but also has a release time in the intestine of 90 to 120 minutes. More importantly, it can increase the flavor and taste of the microcapsule.
  • the present invention also provides a food composition, comprising the intestinal directional release microcapsules described in the above technical solution.
  • the food composition also includes one of a yogurt base, a milk tea base and an acidic milk beverage base, that is, the above-mentioned intestinal directional energy-releasing microcapsules are added to yogurt, milk tea or acidic milk beverage.
  • the present invention has no special content for the components and contents of the yogurt base, milk tea base and acidic milk beverage base, and the raw material combination that can prepare yogurt, milk tea and acidic milk beverage that is well known to those skilled in the art can be used.
  • the present invention has no special restrictions on the content of microcapsules in the food composition, which can be 1wt% to 20wt%, preferably 3wt% to 10wt%.
  • the intestinal directional release microcapsule provided by the present invention is a three-layer packaging structure, which includes a sodium alginate and gelatin layer, a powder coating layer and a glue coating layer.
  • the three-layer structure not only improves the stability of the functional active ingredients, so that it can be applied to room temperature acidic liquid products, but also can be further coated with powder and glue on the outside to enrich the taste of the product, and can be released in the intestine, and the release time in the intestine is 90 to 120 minutes. Further, the microcapsule can be added to room temperature acidic liquid products to enrich the taste of the product and have good acid resistance.
  • FIG1 is a photograph of a single microcapsule provided in an embodiment of the present invention.
  • FIG2 is a photo of a plurality of microcapsules provided in an embodiment of the present invention.
  • FIG3 is a CLSM image of each stage of in vitro dynamic simulated gastrointestinal digestion of three-layer embedded Bacillus coagulans microcapsules at room temperature yogurt;
  • FIG4 is a CLSM image of each stage of in vitro dynamic simulation of gastrointestinal digestion of naked Bacillus coagulans at room temperature yogurt;
  • FIG5 is a statistical graph showing the number of live bacteria at each stage of in vitro dynamic simulated gastrointestinal digestion of room temperature yogurt with three-layer embedded Bacillus coagulans microcapsules.
  • the present invention provides an intestinal directional release microcapsule, a preparation method thereof and a food composition.
  • Those skilled in the art can refer to the content of this article and appropriately improve the process parameters to achieve it. It should be particularly noted that all similar substitutions and modifications are obvious to those skilled in the art, and they are all considered to be included in the present invention.
  • the methods and applications of the present invention have been described through preferred embodiments, and relevant personnel can obviously modify or appropriately change and combine the methods and applications of this article without departing from the content, spirit and scope of the present invention to implement and apply the technology of the present invention.
  • the first layer of wall material is made of gelatin and sodium alginate heated and mixed in a mass ratio of 1:1, and 20wt% of Bacillus coagulans, 70wt% of vegetable oil and 10wt% of emulsifier phospholipids are used as core materials.
  • a dropper with an inner diameter of 1mm and an outer diameter of 1.5mm is used, the inner diameter is filled with the core material solution, and the outer diameter is filled with the wall material solution.
  • the temperature is kept at 80 ⁇ 2°C, the drop rate is controlled at 15 drops/s, the cooling liquid column is 10cm/120cm, and the cooling temperature is 9-12°C. According to the design of 2.7 ⁇ 10 6 CFU/mg microcapsules, circular single-layer embedded Bacillus coagulans microcapsules with a diameter of 3 mm were obtained.
  • the circular single-layer embedded Bacillus coagulans microcapsules are coated with cassava starch to obtain double-layer embedded Bacillus coagulans microcapsules coated with cassava starch.
  • the mass ratio of the circular single-layer embedded Bacillus coagulans microcapsules to cassava starch is 1:3.
  • the double-layer embedded Bacillus coagulans microcapsules are cast in a 5% sodium alginate solution to obtain a three-layer embedded Bacillus coagulans microcapsule wrapped with sodium alginate.
  • the mass ratio of the circular single-layer embedded Bacillus coagulans microcapsules, cassava starch and sodium alginate is 1:3:2.
  • FIG. 1 is a photograph of a single microcapsule provided in an embodiment of the present invention
  • FIG. 2 is a photograph of a plurality of microcapsules provided in an embodiment of the present invention.
  • Embedding rate (%) number of live bacteria embedded in microcapsules / number of live bacteria added when preparing microcapsules ⁇ 100%
  • Table 1 Specific composition of the in vitro dynamic simulated gastrointestinal digestive fluid provided by the embodiment of the present invention
  • the final volume of each simulated digestive solution was 500 mL.
  • CaCl 2 (H 2 O) 2 was added to the gastric and intestinal digestive systems at final concentrations of 0.075 mmol/L and 0.3 mmol/L, respectively, before digestion and mixed directly with the food.
  • the dynamic gastric digestion model was used to simulate gastric digestion in vitro on samples (room temperature yogurt containing three-layer embedded Bacillus coagulans microcapsules and room temperature yogurt containing naked Bacillus coagulans). 133.3 mL of SGF dissolved with pepsin (2000 U/mL) was added into the artificial stomach at a rate of 1.33 mL/min (1-10 min) and 1.09 mL/min (10-120 min), while pH-stat was used to control pH according to the following program: 5.3-4.3 (0-20 min), 4.3-3.6 (20-40 min), 3.6-3.1 (40-70 min), 3.1-2.5 (70-90 min), 2.5 (90-120 min).
  • Gastric emptying rates were: 1.34 mL/min (0-30 min), 1.97 mL/min (30-60 min), 1.64 mL/min (60-90 min), 1.08 mL/min (90-120 min). Samples were taken at 30 min, 60 min, 90 min and 120 min of gastric digestion and stored on ice for subsequent analysis.
  • the formula of room temperature yogurt containing three-layer embedded Bacillus coagulans microcapsules is: 70% raw cow's milk, 10% white sugar, 2% whey protein powder, 120U/T of Chr. Hansen fermentation bacteria, 2.5% pectin, 4% physically modified starch, 1% citrus fiber, and 10% three-layer embedded Bacillus coagulans microcapsules.
  • the formula of room temperature yogurt containing naked Bacillus coagulans is: 75% raw milk, 13% white sugar, 2% whey protein powder, 120U/T of Chr. Hansen fermentation bacteria, 2.5% pectin, 4% physically modified starch, citrus Fiber 1%, Bacillus 2%.
  • the pH of the final product of gastric digestion was adjusted to 7.0, and placed in a simulated small intestinal system (AIDS) for simulated intestinal digestion.
  • 100 mL of SIF dissolved with pancreatic enzymes (pancreatic lipase 2000 U/mL) and bile salts (10 mmol/L) was added to the digestion system at a rate of 0.55 mL/min.
  • the pH of the system was maintained at 7.0 using pH-stat. Digestion was performed for 3 h, and the emptying rates were: 0.47 mL/min (0-85 min), 0.30 mL/min (85-180 min). Samples were taken at 30 min, 60 min, 90 min, and 180 min of intestinal digestion and stored on ice for subsequent analysis.
  • Figure 3 is the CLSM images of the in vitro dynamic simulated gastrointestinal digestion stages of the three-layer embedded Bacillus coagulans microcapsule room temperature yogurt, wherein Figure 3 (A) is the original sample; Figure 3 (B) is the sample after 30 minutes of gastric digestion; Figure 3 (C) is the sample after 60 minutes of gastric digestion; Figure 3 (D) is the sample after 90 minutes of gastric digestion; Figure 3 (E) is the sample after 120 minutes of gastric digestion; Figure 3 (F) is the sample after 30 minutes of intestinal digestion; Figure 3 (G) is the sample after 60 minutes of intestinal digestion; Figure 3 (H) is the sample after 90 minutes of intestinal digestion; Figure 3 (I) is the sample after 120 minutes of intestinal digestion, among which the green fluorescence is the live bacteria, and the red fluorescence is the dead bacteria.
  • Figure 4 is the CLSM images of each stage of in vitro dynamic simulation of gastrointestinal digestion of naked Bacillus coagulans room temperature yogurt, wherein, Figure 4 (A) is the original sample; Figure 4 (B) is the sample after 30 minutes of gastric digestion; Figure 4 (C) is the sample after 60 minutes of gastric digestion; Figure 4 (D) is the sample after 90 minutes of gastric digestion; Figure 4 (E) is the sample after 120 minutes of gastric digestion; Figure 4 (F) is the sample after 30 minutes of intestinal digestion; Figure 4 (G) is the sample after 60 minutes of intestinal digestion; Figure 4 (H) is the sample after 90 minutes of intestinal digestion; Figure 4 (I) is the sample after 120 minutes of intestinal digestion, among which those emitting green fluorescence are live bacteria, and those emitting red fluorescence are dead bacteria.
  • Figure 5 is a statistical graph of the number of live bacteria in each stage of in vitro dynamic simulation of gastrointestinal digestion of three-layer embedded Bacillus coagulans microcapsules room temperature yogurt.
  • the number of live bacteria represented by green fluorescence gradually decreases as the digestion time increases.
  • the reason may be that the live bacteria are intolerant to the effects of gastric acid, resulting in a gradual decrease in the number. It may also be due to the continuous secretion of gastric juice during the dynamic digestion process, thereby diluting the concentration of live bacteria in the digestion products.
  • the fluorescence intensity gradually increases, the three-layer embedded microcapsules begin to degrade and release the inner layer of Bacillus coagulans.
  • the three-layer embedded microcapsules can release Bacillus coagulans in a targeted manner in the small intestine.
  • the three-layer microcapsules can The survival rate of Bacillus coagulans in an acidic environment can be improved. This may be due to the dense structure of the microcapsules, small pore size, high mechanical strength, and the outermost layer of sodium alginate, which is a pH-sensitive gel and is relatively stable at low pH. It can better resist gastric juice penetration, thereby improving the survival rate of Bacillus coagulans.
  • agar, 35wt% gelatin and 35wt% sodium alginate are heated and mixed to form the first layer of wall material, 20wt% of Bacillus coagulans, 60wt% of vegetable oil, 10wt% of emulsifiers propylene glycol fatty acid ester and glycerol fatty acid ester (the mass ratio of propylene glycol fatty acid ester and glycerol fatty acid ester is 1:1) and 10wt% of prebiotics are used as core materials, a dropper with an inner diameter of 1mm and an outer diameter of 1.5mm is used, the inner diameter is filled with the core material solution, and the outer diameter is filled with the wall material solution, the temperature is kept at 80 ⁇ 2°C, the drop rate is controlled at 15 drops/s, the cooling liquid column is 10cm/120cm, the cooling temperature is 9-12°C, and according to the design of 2.7 ⁇ 10 6 CFU/mg microcapsules, a circular single-layer embedded Bacillus coagulans micro
  • the circular single-layer embedded Bacillus coagulans microcapsules are coated with cassava starch to obtain double-layer embedded Bacillus coagulans microcapsules coated with cassava starch.
  • the mass ratio of the circular single-layer embedded Bacillus coagulans microcapsules to cassava starch is 1:3.
  • the double-layer embedded Bacillus coagulans microcapsules are cast in a 5% sodium alginate solution to obtain a three-layer embedded Bacillus coagulans microcapsule wrapped with sodium alginate.
  • the mass ratio of the circular single-layer embedded Bacillus coagulans microcapsules, cassava starch and sodium alginate is 1:3:2.
  • the obtained three-layer embedded Bacillus coagulans microcapsules were immersed in 10 wt % calcium chloride for 60 minutes to obtain solidified microcapsules.
  • Example 2 The difference from Example 2 is that the first layer wall material solution is 70 wt % agar, 15 wt % sodium alginate and 15 wt % gelatin.
  • Example 2 The difference from Example 2 is that the first layer of wall material solution is 70 wt % agar and 30 wt % sodium alginate.
  • Example 2 The microcapsules prepared in Example 2 and Comparative Examples 1-2 were placed at 37°C and the probiotic loss was detected. The results are shown in Table 2. Table 2 shows the probiotic loss detection results of the microcapsules prepared in the Examples of the present invention and Comparative Examples at high temperature.

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Abstract

The present invention provides a microcapsule for intestinal-targeted release, comprising: a core material, the core material comprising an active ingredient; a first wall material layer wrapping the core material, the first wall material layer comprising gelatin and sodium alginate, and the content of the gelatin being at least 20 wt%; a second wrapping layer wrapping the first wall material layer, the second wrapping layer being formed by powdery substances; and a third wrapping layer wrapping the second wrapping layer, the third wrapping layer being formed by gum substances. The microcapsule for intestinal-targeted release provided by the present invention is of a three-layer wrapping structure, which improves the stability of the functional active ingredient, so that the microcapsule can be applied to a normal-temperature acidic liquid product, can further be wrapped with powder and gum to enrich the taste of the product, and can be released in an intestinal tract, and the release time of the microcapsule in the intestinal tract is 90-120 mins.

Description

肠道定向释放微胶囊、其制备方法及食品组合物Intestinal directional release microcapsule, preparation method thereof and food composition
本申请要求于2022年11月30日提交中国国家知识产权局、申请号为202211520367.7、发明名称为“肠道定向释放微胶囊、其制备方法及食品组合物”的中国专利申请的优先权，其全部内容通过引用结合在本申请中。This application claims priority to the Chinese patent application filed with the State Intellectual Property Office of China on November 30, 2022, with application number 202211520367.7 and invention name “Intestinal Targeted Release Microcapsules, Preparation Methods and Food Compositions Thereof”, the entire contents of which are incorporated by reference into this application.
技术领域Technical Field
本发明涉及食品技术领域，尤其涉及一种肠道定向释放微胶囊、其制备方法及食品组合物。The present invention relates to the field of food technology, and in particular to an intestinal directional release microcapsule, a preparation method thereof and a food composition.
背景技术Background technique
微胶囊技术是利用包埋材料将目标芯材(固体、液体甚至气体)包裹，形成一种直径在1～5000μm范围的具有半透性或密封囊膜的微型胶囊。益生菌能产生多种活性物质，在肠道微生态平衡的调控及某些疾病的防治中发挥重要作用。但是，大部分益生菌不耐酸，经过胃液和消化道上端的胆盐环境后，活菌数大幅度下降，会影响产品疗效。将益生菌制成微胶囊是目前解决益生菌耐酸性最有效、最有前景的方法之一，微胶囊可为益生菌提供有效的物理屏障，确保一定数量的益生菌在消化道中存活并在小肠定向释放。Microencapsulation technology uses an embedding material to encapsulate the target core material (solid, liquid or even gas) to form a microcapsule with a diameter ranging from 1 to 5000 μm and a semi-permeable or sealed capsule membrane. Probiotics can produce a variety of active substances and play an important role in regulating the balance of intestinal microecology and preventing and treating certain diseases. However, most probiotics are not acid-resistant. After passing through the gastric juice and bile salt environment at the upper end of the digestive tract, the number of live bacteria drops significantly, which will affect the efficacy of the product. Making probiotics into microcapsules is currently one of the most effective and promising methods to solve the acid resistance of probiotics. Microcapsules can provide an effective physical barrier for probiotics, ensuring that a certain number of probiotics survive in the digestive tract and are released in a targeted manner in the small intestine.
现有技术公开多种微胶囊的包埋方法，例如中国专利CN115039886A公开了一种双歧杆菌微胶囊，其以多孔淀粉为保护剂，将其负载双歧杆菌后，再依次采用黄原胶-海藻糖-酪蛋白-海藻酸钠、果胶-海藻酸钠和玉米醇溶蛋白乙醇溶液进行三次包被，得到三层包裹的微胶囊。该微胶囊虽然耐酸、耐胆盐能力较好，但其在肠道中活菌的释放较为缓慢。The prior art discloses a variety of microcapsule embedding methods. For example, Chinese patent CN115039886A discloses a bifidobacterium microcapsule, which uses porous starch as a protective agent, loads bifidobacteria, and then uses xanthan gum-trehalose-casein-sodium alginate, pectin-sodium alginate and zein alcohol solution for three times of coating to obtain a three-layer coated microcapsule. Although the microcapsule has good acid and bile salt resistance, it releases live bacteria in the intestine slowly.
发明内容Summary of the invention
有鉴于此，本发明要解决的技术问题在于提供一种肠道定向释放微胶囊、其制备方法及食品组合物，本发明提供的肠道定向释放微胶囊耐酸性能好，能够在肠道定向释放，而且在90～120min内释放完全。In view of this, the technical problem to be solved by the present invention is to provide an intestinal directional release microcapsule, a preparation method thereof and a food composition. The intestinal directional release microcapsule provided by the present invention has good acid resistance, can be directed released in the intestine, and can be completely released within 90 to 120 minutes.
本发明提供了一种肠道定向释放微胶囊，包括： The present invention provides an intestinal directional release microcapsule, comprising:
芯材，所述芯材包括活性成分；a core material, the core material comprising an active ingredient;
包裹所述芯材的第一壁材层，所述第一壁材层包括明胶和海藻酸钠，所述明胶的含量至少为20wt％；a first wall material layer wrapping the core material, the first wall material layer comprising gelatin and sodium alginate, wherein the content of the gelatin is at least 20 wt %;
包裹所述第一壁材层的第二包裹层，所述第二包裹层由粉状物质形成；a second wrapping layer wrapping the first wall material layer, wherein the second wrapping layer is formed of a powdery substance;
包裹所述第二包裹层的第三包裹层，所述第三包裹层由胶类物质形成。A third wrapping layer wrapping the second wrapping layer, wherein the third wrapping layer is formed of a glue-like substance.
本发明提供的肠道定向释放微胶囊为三层包裹结构，不仅耐酸性能好，能够在肠道定向释放，而且能够在90～120min内释放。The intestinal directional release microcapsule provided by the present invention has a three-layer packaging structure, which not only has good acid resistance and can be directed to the intestinal tract, but also can be released within 90 to 120 minutes.
在所述微胶囊中，芯材包括活性成分，所述活性成分选自益生菌、益生元、维生素和DHA中的一种或多种，优选为益生菌。所述芯材还包括油脂和乳化剂，其中，油脂可以为植物油，例如椰子油、植物混合油、棕榈油；乳化剂选自多元醇脂肪酸酯类，包括丙二醇脂肪酸酯、甘油脂肪酸酯、糖酯、聚甘油脂肪酸酯、磷脂类、酪蛋白酸钠等。具体而言，所述芯材可以包括：1wt％～99wt％的油脂；1wt％～50wt％的活性成分；和0～20wt％的润滑剂。优选包括：20wt％～80wt％的油脂；10wt％～40wt％的活性成分；和10～20wt％的乳化剂。在一些可能的实现方式中，所述芯材包括20wt％～80wt％的油脂；10wt％～20wt％的益生菌；10wt％～20wt％的益生元和10～20wt％的乳化剂。In the microcapsule, the core material includes an active ingredient, which is selected from one or more of probiotics, prebiotics, vitamins and DHA, preferably probiotics. The core material also includes oils and emulsifiers, wherein the oils can be vegetable oils, such as coconut oil, vegetable mixed oils, and palm oil; the emulsifier is selected from polyol fatty acid esters, including propylene glycol fatty acid esters, glycerol fatty acid esters, sugar esters, polyglycerol fatty acid esters, phospholipids, sodium caseinate, etc. Specifically, the core material may include: 1wt% to 99wt% of oils; 1wt% to 50wt% of active ingredients; and 0 to 20wt% of lubricants. Preferably, it includes: 20wt% to 80wt% of oils; 10wt% to 40wt% of active ingredients; and 10 to 20wt% of emulsifiers. In some possible implementations, the core material includes 20wt% to 80wt% of oils; 10wt% to 20wt% of probiotics; 10wt% to 20wt% of prebiotics and 10 to 20wt% of emulsifiers.
本发明提供的肠道定向释放微胶囊包括包裹所述芯材的第一壁材层，所述第一壁材层包括明胶和海藻酸钠，所述明胶的含量至少为20wt％。明胶和海藻酸钠形成的第一壁材层使得微胶囊囊壁孔隙率较低，从而使得胶囊在90～120min内在肠道内释放。在一些可能的实现方式中，所述明胶和海藻酸钠的质量比为3～10:0.3～5，优选为4～8:1～4。在一些可能的实现方式中，所述第一壁材层还包括琼脂，所述琼脂、明胶和海藻酸钠的质量比为3～15:3～10：0.3～5，更优选为4～10:4～8:1～4。在一些可能的实现方式中，所述芯材与第一壁材的质量比为3：4～6，优选为3:5。在一些可能的实现方式中，所述第一壁材的厚度为1.5～2.5mm，优选为2mm。在一些可能的实现方式中，所述第一壁材层还包括钙化交联剂，使明胶和海藻酸钠形成的壁材固化变硬，得到硬胶囊。所述钙化交联剂包括但不限于氯化钙或乳酸钙，优选为氯化钙。在一些可能的实现方式中，所述钙化交联剂与海藻酸钠的质量比为1:4～6，优选为1：5。在一些可能的实现方式中，包裹第一层壁材的微胶囊的粒径为0.5～15mm，优选为1～10mm，更优选为3～8mm。 The intestinal directional release microcapsule provided by the present invention includes a first wall material layer wrapping the core material, the first wall material layer includes gelatin and sodium alginate, and the content of the gelatin is at least 20wt%. The first wall material layer formed by gelatin and sodium alginate makes the microcapsule wall porosity lower, so that the capsule is released in the intestine within 90 to 120 minutes. In some possible implementations, the mass ratio of gelatin and sodium alginate is 3 to 10: 0.3 to 5, preferably 4 to 8: 1 to 4. In some possible implementations, the first wall material layer also includes agar, and the mass ratio of agar, gelatin and sodium alginate is 3 to 15: 3 to 10: 0.3 to 5, more preferably 4 to 10: 4 to 8: 1 to 4. In some possible implementations, the mass ratio of the core material to the first wall material is 3: 4 to 6, preferably 3: 5. In some possible implementations, the thickness of the first wall material is 1.5 to 2.5 mm, preferably 2 mm. In some possible implementations, the first wall material layer also includes a calcified crosslinking agent to solidify and harden the wall material formed by gelatin and sodium alginate to obtain a hard capsule. The calcified crosslinking agent includes but is not limited to calcium chloride or calcium lactate, preferably calcium chloride. In some possible implementations, the mass ratio of the calcified crosslinking agent to sodium alginate is 1:4 to 6, preferably 1:5. In some possible implementations, the particle size of the microcapsules wrapped in the first layer of wall material is 0.5 to 15 mm, preferably 1 to 10 mm, and more preferably 3 to 8 mm.
本发明提供的肠道定向释放微胶囊包括包裹所述第一壁材层的第二包裹层，所述第二包裹层由粉状物质形成。所述粉状物质一方面为微胶囊提供特定的风味，一方面增加微胶囊的耐酸性，同时不影响微胶囊在肠道中的释放。所述粉状物质包括风味物质粉，例如芝士粉、淀粉、蛋白粉和果粉中的一种或多种；也可以为功能性粉，例如膳食纤维、VC、VB、DHA等营养强化剂，还可以为胶体粉，例如木薯粉。在一些可能的实现方式中，所述第二包裹层的厚度为1.5～2.5mm，优选为2mm。所述第二包裹层和芯材的质量比为1:1.5～3，优选为1：2。The intestinal directional release microcapsules provided by the present invention include a second wrapping layer wrapping the first wall material layer, and the second wrapping layer is formed by a powdery substance. The powdery substance provides a specific flavor for the microcapsules on the one hand, and increases the acid resistance of the microcapsules on the other hand, while not affecting the release of the microcapsules in the intestine. The powdery substance includes flavor substance powder, such as one or more of cheese powder, starch, protein powder and fruit powder; it can also be functional powder, such as dietary fiber, VC, VB, DHA and other nutritional enhancers, and can also be colloidal powder, such as cassava flour. In some possible implementations, the thickness of the second wrapping layer is 1.5 to 2.5 mm, preferably 2 mm. The mass ratio of the second wrapping layer to the core material is 1:1.5 to 3, preferably 1:2.
本发明提供的肠道定向释放微胶囊包括包裹所述第二包裹层的第三包裹层，所述第三包裹层由胶类物质形成。所述胶类物质一方面赋予微胶囊特殊的口感，一方面增加微胶囊的耐酸性，同时不影响微胶囊在肠道中的释放。在一些可能的实现方式中，所述胶类物质选自魔芋胶、卡拉胶、海藻酸钠、结冷胶、羧甲基纤维素钠、黄原胶、琼脂、果胶与明胶中的一种或多种，优选至少包括海藻酸钠。在一些可能的实现方式中，所述第三包裹层的厚度为2～4mm，优选为3mm。所述第三包裹层与所述芯材的质量比为1:2～5，优选为1：4。The intestinal directional release microcapsules provided by the present invention include a third wrapping layer wrapping the second wrapping layer, and the third wrapping layer is formed by a gum-like substance. The gum-like substance gives the microcapsules a special taste on the one hand, and increases the acid resistance of the microcapsules on the other hand, while not affecting the release of the microcapsules in the intestine. In some possible implementations, the gum-like substance is selected from one or more of konjac gum, carrageenan, sodium alginate, gellan gum, sodium carboxymethyl cellulose, xanthan gum, agar, pectin and gelatin, preferably including at least sodium alginate. In some possible implementations, the thickness of the third wrapping layer is 2 to 4 mm, preferably 3 mm. The mass ratio of the third wrapping layer to the core material is 1:2 to 5, preferably 1:4.
本发明提供的微胶囊包括三层壁材，分别为海藻酸钠和明胶层、裹粉层和裹胶层，该三层结构不仅使得微胶囊具有耐酸性，能够在肠道内释放，而且其在肠道内的释放时间为90～120min，更重要的是能够增加微胶囊的风味和口感。The microcapsule provided by the present invention comprises three layers of wall materials, namely a sodium alginate and gelatin layer, a powder coating layer and a gelatin coating layer. The three-layer structure not only makes the microcapsule acid-resistant and can be released in the intestine, but also has a release time in the intestine of 90 to 120 minutes. More importantly, it can increase the flavor and taste of the microcapsule.
本发明还提供了一种上述技术方案所述的肠道定向释放微胶囊的制备方法，包括以下步骤：The present invention also provides a method for preparing the intestinal directional release microcapsules described in the above technical solution, comprising the following steps:
以包括明胶和海藻酸钠的混合物作为第一层壁材包裹包括活性成分的芯材，形成包括芯材和第一壁材层的单层微胶囊；所述混合物中，明胶的含量至少为20wt％；A core material including an active ingredient is encapsulated with a mixture including gelatin and sodium alginate as a first layer of wall material to form a single-layer microcapsule including the core material and the first wall material layer; the content of gelatin in the mixture is at least 20 wt%;
以粉状物质包裹所述单层微胶囊，形成双层包裹的微胶囊；wrapping the single-layer microcapsules with a powdery substance to form double-layer wrapped microcapsules;
以胶类物质包裹所述双层包裹的微胶囊，形成三层包裹的微胶囊。The double-layer wrapped microcapsules are wrapped with a glue-like substance to form triple-layer wrapped microcapsules.
本发明首先将作为壁材的明胶和海藻酸钠加热混合形成壁材溶液，然后将包括活性成分的芯材在壁材溶液中进行滴丸包埋，形成壁材包裹芯材的微胶囊。其中，芯材、壁材的选择及用量如上文所述，本申请在此不再赘述。所述滴丸包埋可采用本领域技术人员熟知的方式，本申请在此不再赘述。The present invention first heats and mixes gelatin and sodium alginate as wall materials to form a wall material solution, and then embeds the core material including the active ingredient in the wall material solution to form a microcapsule in which the wall material encapsulates the core material. The selection and dosage of the core material and the wall material are as described above, and the present application will not repeat them here. The embedding of the drop pills can be carried out in a manner well known to those skilled in the art, and the present application will not repeat them here.
在一些可能的实现方式中，形成壁材包裹芯材的微胶囊后，将其在钙化交 联剂溶液中进行钙化交联，所述钙化交联剂选自氯化钙或乳酸钙。所述钙化交联剂溶液的浓度为1～20wt％，优选为5～15wt％。将微胶囊在钙化交联剂溶液中浸泡30～90min，即可使得壁材固化变硬。In some possible implementations, after the microcapsules with the wall material encapsulating the core material are formed, the microcapsules are placed in a calcified The microcapsules are calcified and cross-linked in a cross-linking agent solution, wherein the cross-linking agent is selected from calcium chloride or calcium lactate. The concentration of the cross-linking agent solution is 1 to 20 wt%, preferably 5 to 15 wt%. The microcapsules are immersed in the cross-linking agent solution for 30 to 90 minutes to solidify the wall material.
包裹第一壁材后，采用粉状物质对得到的单层微胶囊进行第二层包裹。本发明对采用粉状物质对单层微胶囊进行第二层包裹的方法没有特殊限制，将单层微胶囊与粉状物质混合，使粉状物质包裹在单层微胶囊上即可，也可以将粉状物质与水形成悬浊液，与单层微胶囊混合，使粉体包裹在微胶囊外层，干燥即可。After the first wall material is wrapped, the obtained single-layer microcapsules are wrapped with a powdery substance for a second layer. The present invention has no particular limitation on the method of wrapping the single-layer microcapsules with a powdery substance for a second layer. The single-layer microcapsules can be mixed with the powdery substance to wrap the powdery substance on the single-layer microcapsules. Alternatively, the powdery substance can be mixed with water to form a suspension, mixed with the single-layer microcapsules, and the powdery substance can be wrapped on the outer layer of the microcapsules, and then dried.
包裹第二层后，采用胶类物质对得到的双层微胶囊进行第三层包裹。本发明对采用胶类物质对双层微胶囊进行第三层包裹的方法没有特殊限制，将双层微胶囊与胶类物质溶液混合，使胶类物质包裹在双层微胶囊表面，干燥后即可形成第三层。After the second layer is wrapped, the obtained double-layer microcapsules are wrapped with a glue-like substance for a third layer. The present invention has no special restrictions on the method of wrapping the double-layer microcapsules with a glue-like substance for a third layer. The double-layer microcapsules are mixed with a glue-like substance solution, and the glue-like substance is wrapped on the surface of the double-layer microcapsules. After drying, the third layer can be formed.
制备得到微胶囊后，还可以将其制备成料酱，所述料酱包括水、甜味剂和上述微胶囊，所述料酱的pH值为酸性。具体而言，首先将水与甜味剂混合，将得到的混合液的pH值调节至酸性，与上述微胶囊混合后灭菌，即可得到料酱。在一些具体的实现方式中，所述灭菌的温度为65℃～121℃，优选为70℃～115℃，更优选为80℃～100℃；灭菌的时间为4s～30min，优选为1min～25min，更优选为5min～20min。本发明对所述料酱中微胶囊的含量没有特殊限制，可以为5wt％～80wt％，优选为10wt％～70wt％。本发明对所述甜味剂没有特殊限制，白砂糖、果糖、乳糖等具有甜味的成分即可。After the microcapsules are prepared, they can also be prepared into a sauce, which includes water, a sweetener and the above-mentioned microcapsules, and the pH value of the sauce is acidic. Specifically, water and a sweetener are first mixed, the pH value of the obtained mixed solution is adjusted to acidic, and the mixture is sterilized after mixing with the above-mentioned microcapsules to obtain a sauce. In some specific implementations, the sterilization temperature is 65°C to 121°C, preferably 70°C to 115°C, and more preferably 80°C to 100°C; the sterilization time is 4s to 30min, preferably 1min to 25min, and more preferably 5min to 20min. The present invention has no special restrictions on the content of microcapsules in the sauce, which can be 5wt% to 80wt%, preferably 10wt% to 70wt%. The present invention has no special restrictions on the sweetener, and white sugar, fructose, lactose and other sweet ingredients can be used.
本发明提供的微胶囊包括三层壁材，分别为海藻酸钠和明胶层、裹粉层和裹胶层，该三层结构不仅使得微胶囊具有耐酸性，能够在肠道内释放，而且其在肠道内的释放时间为90～120min，更重要的是能够增加微胶囊的风味和口感。The microcapsule provided by the present invention comprises three layers of wall materials, namely a sodium alginate and gelatin layer, a powder coating layer and a gelatin coating layer. The three-layer structure not only makes the microcapsule acid-resistant and can be released in the intestine, but also has a release time in the intestine of 90 to 120 minutes. More importantly, it can increase the flavor and taste of the microcapsule.
本发明还提供了一种食品组合物，包括上述技术方案所述的肠道定向释放微胶囊。在一些具体的实现方式中，所述食品组合物还包括酸奶基料、奶茶基料和酸性乳饮料基料中的一种，即在酸奶、奶茶或酸性乳饮料中添加上述肠道定向能释放微胶囊。本发明对所述酸奶基料、奶茶基料和酸性乳饮料基料的组分及其含量没有特殊含量，本领域技术人员熟知的能够制备得到酸奶、奶茶和酸性乳饮料的原料组合即可。本发明对所述食品组合物中微胶囊的含量没有特殊限制，可以为1wt％～20wt％，优选为3wt％～10wt％。 The present invention also provides a food composition, comprising the intestinal directional release microcapsules described in the above technical solution. In some specific implementations, the food composition also includes one of a yogurt base, a milk tea base and an acidic milk beverage base, that is, the above-mentioned intestinal directional energy-releasing microcapsules are added to yogurt, milk tea or acidic milk beverage. The present invention has no special content for the components and contents of the yogurt base, milk tea base and acidic milk beverage base, and the raw material combination that can prepare yogurt, milk tea and acidic milk beverage that is well known to those skilled in the art can be used. The present invention has no special restrictions on the content of microcapsules in the food composition, which can be 1wt% to 20wt%, preferably 3wt% to 10wt%.
本发明提供的肠道定向释放微胶囊为三层包裹结构，分别为海藻酸钠和明胶层、裹粉层和裹胶层，该三层结构不仅提高了功能性活性成分的稳定性，使其可应用于常温酸性液态产品，还可以进一步在外面进行裹粉与裹胶，丰富产品的口感，而且能够在肠道内释放，且其在肠道内的释放时间为90～120min。进一步的，该微胶囊可以添加到常温酸性液态产品中，丰富产品的口感，而且具有良好的耐酸性能。The intestinal directional release microcapsule provided by the present invention is a three-layer packaging structure, which includes a sodium alginate and gelatin layer, a powder coating layer and a glue coating layer. The three-layer structure not only improves the stability of the functional active ingredients, so that it can be applied to room temperature acidic liquid products, but also can be further coated with powder and glue on the outside to enrich the taste of the product, and can be released in the intestine, and the release time in the intestine is 90 to 120 minutes. Further, the microcapsule can be added to room temperature acidic liquid products to enrich the taste of the product and have good acid resistance.
附图说明BRIEF DESCRIPTION OF THE DRAWINGS
图1为本发明实施例提供的单个微胶囊的照片；FIG1 is a photograph of a single microcapsule provided in an embodiment of the present invention;
图2为本发明实施例提供的多个微胶囊的照片；FIG2 is a photo of a plurality of microcapsules provided in an embodiment of the present invention;
图3为三层包埋凝结芽孢杆菌微胶囊常温酸奶的体外动态模拟胃肠消化各阶段CLSM图；FIG3 is a CLSM image of each stage of in vitro dynamic simulated gastrointestinal digestion of three-layer embedded Bacillus coagulans microcapsules at room temperature yogurt;
图4为凝结芽孢杆菌裸菌常温酸奶体外动态模拟胃肠消化各阶段CLSM图；FIG4 is a CLSM image of each stage of in vitro dynamic simulation of gastrointestinal digestion of naked Bacillus coagulans at room temperature yogurt;
图5为三层包埋凝结芽孢杆菌微胶囊常温酸奶的体外动态模拟胃肠消化各阶段的活菌数统计图。FIG5 is a statistical graph showing the number of live bacteria at each stage of in vitro dynamic simulated gastrointestinal digestion of room temperature yogurt with three-layer embedded Bacillus coagulans microcapsules.
具体实施方式Detailed ways
本发明提供了一种肠道定向释放微胶囊、其制备方法及食品组合物，本领域技术人员可以借鉴本文内容，适当改进工艺参数实现。特别需要指出的是，所有类似的替换和改动对本领域技术人员来说是显而易见的，它们都被视为包括在本发明。本发明的方法及应用已经通过较佳实施例进行了描述，相关人员明显能在不脱离本发明内容、精神和范围内对本文的方法和应用进行改动或适当变更与组合，来实现和应用本发明技术。The present invention provides an intestinal directional release microcapsule, a preparation method thereof and a food composition. Those skilled in the art can refer to the content of this article and appropriately improve the process parameters to achieve it. It should be particularly noted that all similar substitutions and modifications are obvious to those skilled in the art, and they are all considered to be included in the present invention. The methods and applications of the present invention have been described through preferred embodiments, and relevant personnel can obviously modify or appropriately change and combine the methods and applications of this article without departing from the content, spirit and scope of the present invention to implement and apply the technology of the present invention.
实施例1Example 1
(1)三层包埋凝结芽孢杆菌微胶囊的制备(1) Preparation of three-layer microcapsules encapsulating Bacillus coagulans
以质量比为1:1的明胶与海藻酸钠加热混合后为第一层壁材，以20wt％的凝结芽孢杆菌、70wt％的植物油和10wt％的乳化剂磷脂为芯材，采用内径1mm、外径1.5mm滴管，内径中充满芯材溶液，外径中充满壁材溶液，80±2℃保温滴制，滴速控制在15滴/s，冷却液柱10cm/120cm，冷却温度在9-12℃， 按照2.7×106CFU/mg微胶囊设计，得到直径为3mm圆形单层包埋凝结芽孢杆菌微胶囊。The first layer of wall material is made of gelatin and sodium alginate heated and mixed in a mass ratio of 1:1, and 20wt% of Bacillus coagulans, 70wt% of vegetable oil and 10wt% of emulsifier phospholipids are used as core materials. A dropper with an inner diameter of 1mm and an outer diameter of 1.5mm is used, the inner diameter is filled with the core material solution, and the outer diameter is filled with the wall material solution. The temperature is kept at 80±2℃, the drop rate is controlled at 15 drops/s, the cooling liquid column is 10cm/120cm, and the cooling temperature is 9-12℃. According to the design of 2.7×10 6 CFU/mg microcapsules, circular single-layer embedded Bacillus coagulans microcapsules with a diameter of 3 mm were obtained.
将所述圆形单层包埋凝结芽孢杆菌微胶囊在木薯淀粉中裹粉，得到木薯淀粉包裹的双层包埋凝结芽孢杆菌微胶囊。所述双层包埋凝结芽孢杆菌微胶囊中，所述圆形单层包埋凝结芽孢杆菌微胶囊与木薯淀粉的质量比1：3。The circular single-layer embedded Bacillus coagulans microcapsules are coated with cassava starch to obtain double-layer embedded Bacillus coagulans microcapsules coated with cassava starch. In the double-layer embedded Bacillus coagulans microcapsules, the mass ratio of the circular single-layer embedded Bacillus coagulans microcapsules to cassava starch is 1:3.
最后将所述双层包埋凝结芽孢杆菌微胶囊在5％海藻酸钠溶液中流延成型，得到海藻酸钠包裹的三层包埋凝结芽孢杆菌微胶囊。所述三层包埋凝结芽孢杆菌微胶囊中，所述圆形单层包埋凝结芽孢杆菌微胶囊、木薯淀粉和海藻酸钠的质量比1：3：2。Finally, the double-layer embedded Bacillus coagulans microcapsules are cast in a 5% sodium alginate solution to obtain a three-layer embedded Bacillus coagulans microcapsule wrapped with sodium alginate. In the three-layer embedded Bacillus coagulans microcapsules, the mass ratio of the circular single-layer embedded Bacillus coagulans microcapsules, cassava starch and sodium alginate is 1:3:2.
参见图1和图2，图1为本发明实施例提供的单个微胶囊的照片，图2为本发明实施例提供的多个微胶囊的照片。Referring to FIG. 1 and FIG. 2 , FIG. 1 is a photograph of a single microcapsule provided in an embodiment of the present invention, and FIG. 2 is a photograph of a plurality of microcapsules provided in an embodiment of the present invention.
(2)三层包埋凝结芽孢杆菌微胶囊包埋率测定(2) Determination of the encapsulation efficiency of three-layer encapsulated Bacillus coagulans microcapsules
称取样品1g，置于9mL灭菌蛋白胨水中，37℃恒温振荡，经过一系列10倍梯度稀释后，取合适稀释度的菌悬液于GYE琼脂培养基进行培养，确定活菌数量，按照公式(1)计算包埋率：Weigh 1 g of sample and place it in 9 mL of sterile peptone water. Oscillate at 37°C. After a series of 10-fold gradient dilutions, take the bacterial suspension with appropriate dilutions and culture it on GYE agar medium. Determine the number of live bacteria and calculate the embedding rate according to formula (1):
包埋率(％)＝微胶囊中包埋的活菌数/制备微胶囊时添加的活菌数×100％Embedding rate (%) = number of live bacteria embedded in microcapsules / number of live bacteria added when preparing microcapsules × 100%
公式(1)Formula 1)
(3)三层包埋凝结芽孢杆菌微胶囊常温酸奶体外动态模拟胃肠消化研究(3) Study on the dynamic simulation of gastrointestinal digestion of yogurt at room temperature by three-layer encapsulated Bacillus coagulans microcapsules
①模拟消化液的配制① Preparation of simulated digestive fluid
配制模拟胃液(SGF)和模拟肠液(SIF)，置于-20℃冰箱待用，具体配方见表1，表1为本发明实施例提供的体外动态模拟胃肠消化液的具体组成。 Prepare simulated gastric fluid (SGF) and simulated intestinal fluid (SIF), and place them in a -20°C refrigerator for use. The specific formula is shown in Table 1, which shows the specific composition of the in vitro dynamic simulated gastrointestinal digestive fluid provided in an embodiment of the present invention.
表1本发明实施例提供的体外动态模拟胃肠消化液的具体组成
Table 1 Specific composition of the in vitro dynamic simulated gastrointestinal digestive fluid provided by the embodiment of the present invention
注：每种模拟消化液的最终体积为500mL，为防止Ca2+形成沉淀，CaCl2(H2O)2在进行消化前分别以0.075mmol/L和0.3mmol/L最终浓度加入胃、肠消化体系中，直接与食物混合。Note: The final volume of each simulated digestive solution was 500 mL. To prevent Ca 2+ from forming precipitation, CaCl 2 (H 2 O) 2 was added to the gastric and intestinal digestive systems at final concentrations of 0.075 mmol/L and 0.3 mmol/L, respectively, before digestion and mixed directly with the food.
②动态模拟胃消化② Dynamic simulation of gastric digestion
采用动态胃消化模型(AGDS)对样品(含三层包埋凝结芽孢杆菌微胶囊常温酸奶和含凝结芽孢杆菌裸菌常温酸奶对照样品)进行体外模拟胃消化。将133.3mL溶有胃蛋白酶(2000U/mL)的SGF以1.33mL/min(1～10min)和1.09mL/min(10～120min)的速度加入至人工胃中，同时用pH-stat控制pH按照以下程序进行：5.3～4.3(0-20min)、4.3～3.6(20-40min)、3.6～3.1(40-70min)、3.1～2.5(70-90min)、2.5(90-120min)。胃排空速度为：1.34mL/min(0-30min)、1.97mL/min(30-60min)、1.64mL/min(60-90min)、1.08mL/min(90-120min)。在胃消化30min、60min、90min和120min取样，于冰上储存待后续分析。The dynamic gastric digestion model (AGDS) was used to simulate gastric digestion in vitro on samples (room temperature yogurt containing three-layer embedded Bacillus coagulans microcapsules and room temperature yogurt containing naked Bacillus coagulans). 133.3 mL of SGF dissolved with pepsin (2000 U/mL) was added into the artificial stomach at a rate of 1.33 mL/min (1-10 min) and 1.09 mL/min (10-120 min), while pH-stat was used to control pH according to the following program: 5.3-4.3 (0-20 min), 4.3-3.6 (20-40 min), 3.6-3.1 (40-70 min), 3.1-2.5 (70-90 min), 2.5 (90-120 min). Gastric emptying rates were: 1.34 mL/min (0-30 min), 1.97 mL/min (30-60 min), 1.64 mL/min (60-90 min), 1.08 mL/min (90-120 min). Samples were taken at 30 min, 60 min, 90 min and 120 min of gastric digestion and stored on ice for subsequent analysis.
其中，含三层包埋凝结芽孢杆菌微胶囊常温酸奶的配方为：生牛乳70％、白砂糖10％、乳清蛋白粉2％、科汉森发酵菌种120U/T、果胶2.5％、物理变性淀粉4％、柑橘纤维1％、三层包埋凝结芽孢杆菌微胶囊10％。Among them, the formula of room temperature yogurt containing three-layer embedded Bacillus coagulans microcapsules is: 70% raw cow's milk, 10% white sugar, 2% whey protein powder, 120U/T of Chr. Hansen fermentation bacteria, 2.5% pectin, 4% physically modified starch, 1% citrus fiber, and 10% three-layer embedded Bacillus coagulans microcapsules.
含凝结芽孢杆菌裸菌常温酸奶的配方为：生牛乳75％、白砂糖13％、乳清蛋白粉2％、科汉森发酵菌种120U/T、果胶2.5％、物理变性淀粉4％、柑橘 纤维1％、芽孢杆菌2％。The formula of room temperature yogurt containing naked Bacillus coagulans is: 75% raw milk, 13% white sugar, 2% whey protein powder, 120U/T of Chr. Hansen fermentation bacteria, 2.5% pectin, 4% physically modified starch, citrus Fiber 1%, Bacillus 2%.
③动态模拟肠消化③Dynamic simulation of intestinal digestion
调节胃消化终产物pH至7.0，置于模拟小肠系统(AIDS)进行模拟肠消化，将100mL溶有胰酶(胰脂肪酶2000U/mL)和胆盐(10mmol/L)的SIF以0.55mL/min的速度加入消化体系，用pH-stat控制体系pH维持在7.0，消化3h，排空速度为：0.47mL/min(0-85min)、0.30mL/min(85-180min)。在肠消化30min、60min、90min和180min取样，于冰上储存待后续分析。The pH of the final product of gastric digestion was adjusted to 7.0, and placed in a simulated small intestinal system (AIDS) for simulated intestinal digestion. 100 mL of SIF dissolved with pancreatic enzymes (pancreatic lipase 2000 U/mL) and bile salts (10 mmol/L) was added to the digestion system at a rate of 0.55 mL/min. The pH of the system was maintained at 7.0 using pH-stat. Digestion was performed for 3 h, and the emptying rates were: 0.47 mL/min (0-85 min), 0.30 mL/min (85-180 min). Samples were taken at 30 min, 60 min, 90 min, and 180 min of intestinal digestion and stored on ice for subsequent analysis.
(4)实验结果如下：(4) The experimental results are as follows:
①三层包埋凝结芽孢杆菌微胶囊常温酸奶体外动态模拟胃肠消化微观结构变化① Dynamic simulation of gastrointestinal digestion microstructure changes of three-layer encapsulated Bacillus coagulans microcapsules in room temperature yogurt in vitro
参见图3、图4和图5，图3为三层包埋凝结芽孢杆菌微胶囊常温酸奶的体外动态模拟胃肠消化各阶段CLSM图，其中，图3(A)为原始样品；图3(B)为胃消化30min后的样品；图3(C)为胃消化60min后的样品；图3(D)为胃消化90min后的样品；图3(E)为胃消化120min后的样品；图3(F)为肠消化30min后的样品；图3(G)为肠消化60min后的样品；图3(H)为肠消化90min后的样品；图3(I)为肠消化120min后的样品，其中发绿色荧光的为活菌，红色荧光的为死菌。图4为凝结芽孢杆菌裸菌常温酸奶体外动态模拟胃肠消化各阶段CLSM图，其中，图4(A)为原始样品；图4(B)为胃消化30min后的样品；图4(C)为胃消化60min后的样品；图4(D)为胃消化90min后的样品；图4(E)为胃消化120min后的样品；图4(F)为肠消化30min后的样品；图4(G)为肠消化60min后的样品；图4(H)为肠消化90min后的样品；图4(I)为肠消化120min后的样品，其中发绿色荧光的为活菌，红色荧光的为死菌，图5为三层包埋凝结芽孢杆菌微胶囊常温酸奶的体外动态模拟胃肠消化各阶段的活菌数统计图。See Figures 3, 4 and 5, Figure 3 is the CLSM images of the in vitro dynamic simulated gastrointestinal digestion stages of the three-layer embedded Bacillus coagulans microcapsule room temperature yogurt, wherein Figure 3 (A) is the original sample; Figure 3 (B) is the sample after 30 minutes of gastric digestion; Figure 3 (C) is the sample after 60 minutes of gastric digestion; Figure 3 (D) is the sample after 90 minutes of gastric digestion; Figure 3 (E) is the sample after 120 minutes of gastric digestion; Figure 3 (F) is the sample after 30 minutes of intestinal digestion; Figure 3 (G) is the sample after 60 minutes of intestinal digestion; Figure 3 (H) is the sample after 90 minutes of intestinal digestion; Figure 3 (I) is the sample after 120 minutes of intestinal digestion, among which the green fluorescence is the live bacteria, and the red fluorescence is the dead bacteria. Figure 4 is the CLSM images of each stage of in vitro dynamic simulation of gastrointestinal digestion of naked Bacillus coagulans room temperature yogurt, wherein, Figure 4 (A) is the original sample; Figure 4 (B) is the sample after 30 minutes of gastric digestion; Figure 4 (C) is the sample after 60 minutes of gastric digestion; Figure 4 (D) is the sample after 90 minutes of gastric digestion; Figure 4 (E) is the sample after 120 minutes of gastric digestion; Figure 4 (F) is the sample after 30 minutes of intestinal digestion; Figure 4 (G) is the sample after 60 minutes of intestinal digestion; Figure 4 (H) is the sample after 90 minutes of intestinal digestion; Figure 4 (I) is the sample after 120 minutes of intestinal digestion, among which those emitting green fluorescence are live bacteria, and those emitting red fluorescence are dead bacteria. Figure 5 is a statistical graph of the number of live bacteria in each stage of in vitro dynamic simulation of gastrointestinal digestion of three-layer embedded Bacillus coagulans microcapsules room temperature yogurt.
由图3可知，在胃消化阶段，绿色荧光代表的活菌数量随消化时间延长而逐渐减少，原因可能是活菌不耐受胃酸影响导致数量逐渐降低，还可能是动态消化过程中胃液不断分泌从而稀释了消化产物中的活菌浓度所致。而在肠消化60min到90min阶段，可看到随着荧光强度逐渐增强，三层包埋微胶囊开始降解并释放内层凝结芽孢杆菌，在肠消化90min到120min阶段，活菌数量明显增加，表明三层包埋微胶囊可在小肠定向释放凝结芽孢杆菌。三层微胶囊可 提高凝结芽孢杆菌在酸性环境中的存活率，这可能是由于微胶囊结构致密，孔径较少，机械强度高，最外层海藻酸钠是一种pH敏感性凝胶,在低p H下较为稳定，能较好地抵御胃液渗透，从而可以提高凝结芽孢杆菌的存活率。As shown in Figure 3, during the gastric digestion stage, the number of live bacteria represented by green fluorescence gradually decreases as the digestion time increases. The reason may be that the live bacteria are intolerant to the effects of gastric acid, resulting in a gradual decrease in the number. It may also be due to the continuous secretion of gastric juice during the dynamic digestion process, thereby diluting the concentration of live bacteria in the digestion products. During the 60-90 minute stage of intestinal digestion, it can be seen that as the fluorescence intensity gradually increases, the three-layer embedded microcapsules begin to degrade and release the inner layer of Bacillus coagulans. During the 90-120 minute stage of intestinal digestion, the number of live bacteria increases significantly, indicating that the three-layer embedded microcapsules can release Bacillus coagulans in a targeted manner in the small intestine. The three-layer microcapsules can The survival rate of Bacillus coagulans in an acidic environment can be improved. This may be due to the dense structure of the microcapsules, small pore size, high mechanical strength, and the outermost layer of sodium alginate, which is a pH-sensitive gel and is relatively stable at low pH. It can better resist gastric juice penetration, thereby improving the survival rate of Bacillus coagulans.
由图4可以观察到，随着凝结芽孢杆菌裸菌常温酸奶消化时间的延长，绿色荧光强度逐渐下降，在胃消化阶段活菌数量有比较明显的下降趋势，由原始的聚集状态转变为较为分散的状态。CLSM观察到的现象与所测活菌数结果一致(图5)，在模拟胃消化阶段含凝结芽孢杆菌裸菌常温酸奶中的活菌数下降近5％，而在模拟小肠消化阶段，活菌数量下降趋势减慢，无显著差异，这可能是由于小肠液的动态分泌不断稀释了消化产物中细菌的浓度，但因为肠道内环境为中性，所以对细菌的存活的影响相比胃中的酸性环境要低。It can be observed from Figure 4 that as the digestion time of naked Bacillus coagulans at room temperature yogurt increases, the green fluorescence intensity gradually decreases, and the number of live bacteria has a relatively obvious downward trend in the gastric digestion stage, changing from the original aggregated state to a more dispersed state. The phenomenon observed by CLSM is consistent with the measured live bacteria count results (Figure 5). In the simulated gastric digestion stage, the number of live bacteria in the room temperature yogurt containing naked Bacillus coagulans decreased by nearly 5%, while in the simulated small intestinal digestion stage, the downward trend of the number of live bacteria slowed down, with no significant difference. This may be due to the dynamic secretion of small intestinal fluid that continuously dilutes the concentration of bacteria in the digestion products, but because the intestinal environment is neutral, the impact on bacterial survival is lower than that in the acidic environment of the stomach.
实施例2Example 2
以30wt％的琼脂、35wt％的明胶与35wt％的海藻酸钠加热混合后为第一层壁材，以20wt％的凝结芽孢杆菌、60wt％的植物油、10wt％的乳化剂丙二醇脂肪酸酯和甘油脂肪酸酯(丙二醇脂肪酸酯和甘油脂肪酸酯的质量比为1:1)和10wt％的益生元为芯材，采用内径1mm、外径1.5mm滴管，内径中充满芯材溶液，外径中充满壁材溶液，80±2℃保温滴制，滴速控制在15滴/s，冷却液柱10cm/120cm，冷却温度在9-12℃，按照2.7×106CFU/mg微胶囊设计，得到直径为3mm圆形单层包埋凝结芽孢杆菌微胶囊。30wt% agar, 35wt% gelatin and 35wt% sodium alginate are heated and mixed to form the first layer of wall material, 20wt% of Bacillus coagulans, 60wt% of vegetable oil, 10wt% of emulsifiers propylene glycol fatty acid ester and glycerol fatty acid ester (the mass ratio of propylene glycol fatty acid ester and glycerol fatty acid ester is 1:1) and 10wt% of prebiotics are used as core materials, a dropper with an inner diameter of 1mm and an outer diameter of 1.5mm is used, the inner diameter is filled with the core material solution, and the outer diameter is filled with the wall material solution, the temperature is kept at 80±2℃, the drop rate is controlled at 15 drops/s, the cooling liquid column is 10cm/120cm, the cooling temperature is 9-12℃, and according to the design of 2.7×10 6 CFU/mg microcapsules, a circular single-layer embedded Bacillus coagulans microcapsule with a diameter of 3mm is obtained.
将所述圆形单层包埋凝结芽孢杆菌微胶囊在木薯淀粉中裹粉，得到木薯淀粉包裹的双层包埋凝结芽孢杆菌微胶囊。所述双层包埋凝结芽孢杆菌微胶囊中，所述圆形单层包埋凝结芽孢杆菌微胶囊与木薯淀粉的质量比1：3。The circular single-layer embedded Bacillus coagulans microcapsules are coated with cassava starch to obtain double-layer embedded Bacillus coagulans microcapsules coated with cassava starch. In the double-layer embedded Bacillus coagulans microcapsules, the mass ratio of the circular single-layer embedded Bacillus coagulans microcapsules to cassava starch is 1:3.
最后将所述双层包埋凝结芽孢杆菌微胶囊在5％海藻酸钠溶液中流延成型，得到海藻酸钠包裹的三层包埋凝结芽孢杆菌微胶囊。所述三层包埋凝结芽孢杆菌微胶囊中，所述圆形单层包埋凝结芽孢杆菌微胶囊、木薯淀粉和海藻酸钠的质量比1：3：2。Finally, the double-layer embedded Bacillus coagulans microcapsules are cast in a 5% sodium alginate solution to obtain a three-layer embedded Bacillus coagulans microcapsule wrapped with sodium alginate. In the three-layer embedded Bacillus coagulans microcapsules, the mass ratio of the circular single-layer embedded Bacillus coagulans microcapsules, cassava starch and sodium alginate is 1:3:2.
将得到的三层包埋凝结芽孢杆菌微胶囊在浓度为10wt％的氯化钙中浸泡60min，得到固化的微胶囊。The obtained three-layer embedded Bacillus coagulans microcapsules were immersed in 10 wt % calcium chloride for 60 minutes to obtain solidified microcapsules.
对比例1Comparative Example 1
与实施例2的区别在于，第一层壁材溶液为70wt％的琼脂、15wt％的海藻酸钠和15wt％的明胶。 The difference from Example 2 is that the first layer wall material solution is 70 wt % agar, 15 wt % sodium alginate and 15 wt % gelatin.
对比例2Comparative Example 2
与实施例2的区别在于，第一层壁材溶液为70wt％的琼脂、30wt％的海藻酸钠。The difference from Example 2 is that the first layer of wall material solution is 70 wt % agar and 30 wt % sodium alginate.
将实施例2、对比例1～2制备的微胶囊在37℃下放置，并检测其益生菌损耗量，结果参见表2，表2为本发明实施例及比较例制备的微胶囊高温下益生菌损耗量检测结果。The microcapsules prepared in Example 2 and Comparative Examples 1-2 were placed at 37°C and the probiotic loss was detected. The results are shown in Table 2. Table 2 shows the probiotic loss detection results of the microcapsules prepared in the Examples of the present invention and Comparative Examples at high temperature.
表2本发明实施例及比较例制备的微胶囊高温下益生菌损耗量检测结果(单位CFU/g，37℃)
Table 2 Test results of probiotic loss of microcapsules prepared in the embodiments of the present invention and the comparative examples at high temperature (unit: CFU/g, 37°C)
由表2可知，第一层壁材的选择会影响微胶囊在37℃下被包裹的益生菌的损耗量。It can be seen from Table 2 that the choice of the first layer wall material will affect the loss of probiotics encapsulated in the microcapsules at 37°C.
以上仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。 The above are only preferred embodiments of the present invention. It should be pointed out that, for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principles of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims (11)

  1. 一种肠道定向释放微胶囊，其特征在于，包括：An intestinal directional release microcapsule, characterized by comprising:
    芯材，所述芯材包括活性成分；a core material, the core material comprising an active ingredient;
    包裹所述芯材的第一壁材层，所述第一壁材层包括明胶和海藻酸钠，所述明胶的含量至少为20wt％；a first wall material layer wrapping the core material, the first wall material layer comprising gelatin and sodium alginate, wherein the content of the gelatin is at least 20 wt %;
    包裹所述第一壁材层的第二包裹层，所述第二包裹层由粉状物质形成；a second wrapping layer wrapping the first wall material layer, wherein the second wrapping layer is formed of a powdery substance;
    包裹所述第二包裹层的第三包裹层，所述第三包裹层由胶类物质形成。A third wrapping layer wrapping the second wrapping layer, wherein the third wrapping layer is formed of a glue-like substance.
  2. 根据权利要求1所述的肠道定向释放微胶囊，其特征在于，所述芯材包括活性成分、油脂和乳化剂，所述活性成分选自益生菌、益生元、维生素和DHA中的一种或多种。The intestinal directional release microcapsule according to claim 1 is characterized in that the core material comprises active ingredients, oils and emulsifiers, and the active ingredients are selected from one or more of probiotics, prebiotics, vitamins and DHA.
  3. 根据权利要求1所述的肠道定向释放微胶囊，其特征在于，所述第一壁材层包括琼脂、明胶和海藻酸钠，所述琼脂、明胶和海藻酸钠的质量比为3～15:3～10:0.3～5。The intestinal directional release microcapsule according to claim 1 is characterized in that the first wall material layer comprises agar, gelatin and sodium alginate, and the mass ratio of agar, gelatin and sodium alginate is 3-15:3-10:0.3-5.
  4. 根据权利要求1所述的肠道定向释放微胶囊，其特征在于，所述第一壁材层包括明胶和海藻酸钠，所述明胶和海藻酸钠的质量比为3～10:0.3～5。The intestinal directional release microcapsule according to claim 1 is characterized in that the first wall material layer comprises gelatin and sodium alginate, and the mass ratio of gelatin to sodium alginate is 3-10:0.3-5.
  5. 根据权利要求1所述的肠道定向释放微胶囊，其特征在于，所述粉状物质选自芝士粉、淀粉、蛋白粉和果粉中的一种或多种。The intestinal directional release microcapsule according to claim 1, characterized in that the powdery substance is selected from one or more of cheese powder, starch, protein powder and fruit powder.
  6. 根据权利要求1所述的肠道定向释放微胶囊，其特征在于，所述胶类物质选自魔芋胶、卡拉胶、海藻酸钠、结冷胶、羧甲基纤维素钠、黄原胶、琼脂、果胶与明胶中的一种或多种。The intestinal directional release microcapsule according to claim 1, characterized in that the gum substance is selected from one or more of konjac gum, carrageenan, sodium alginate, gellan gum, sodium carboxymethyl cellulose, xanthan gum, agar, pectin and gelatin.
  7. 根据权利要求1所述的肠道定向释放微胶囊，其特征在于，所述芯材、第一壁材层、第二包裹层和第三包裹层的质量比为：1：2～3：4～5。The intestinal directional release microcapsule according to claim 1 is characterized in that the mass ratio of the core material, the first wall material layer, the second wrapping layer and the third wrapping layer is: 1:2~3:4~5.
  8. 根据权利要求1～7任意一项所述的肠道定向释放微胶囊，其特征在于，所述第一壁材层还包括钙化交联剂；The intestinal directional release microcapsule according to any one of claims 1 to 7, characterized in that the first wall material layer further comprises a calcified cross-linking agent;
    所述钙化交联剂选自氯化钙或乳酸钙。The calcified cross-linking agent is selected from calcium chloride or calcium lactate.
  9. 权利要求1～8任意一项所述的肠道定向释放微胶囊的制备方法，包括以下步骤：The method for preparing the intestinal directional release microcapsules according to any one of claims 1 to 8 comprises the following steps:
    以包括明胶和海藻酸钠的混合物作为第一次壁材包裹包括活性成分的芯材，形成包括芯材和第一壁材层的单层微胶囊；所述混合物中，明胶的含量至 少为20wt％；A core material including an active ingredient is encapsulated with a mixture including gelatin and sodium alginate as a first wall material to form a single-layer microcapsule including a core material and a first wall material layer; in the mixture, the content of gelatin is at least At least 20wt%;
    以粉状物质包裹所述单层微胶囊，形成双层包裹的微胶囊；wrapping the single-layer microcapsules with a powdery substance to form double-layer wrapped microcapsules;
    以胶类物质包裹所述双层包裹的微胶囊，形成三层包裹的微胶囊。The double-layer wrapped microcapsules are wrapped with a glue-like substance to form triple-layer wrapped microcapsules.
  10. 一种食品组合物，包括权利要求1～9任意一项所述的肠道定向释放微胶囊。A food composition comprising the intestinal directional release microcapsule according to any one of claims 1 to 9.
  11. 根据权利要求10所述的食品组合物，其特征在于，还包括酸奶基料、奶茶基料和酸性乳饮料基料中的一种。 The food composition according to claim 10, characterized in that it also includes one of a yogurt base, a milk tea base and an acidic milk beverage base.
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