CN114431466A - Procyanidine microcapsule and preparation method thereof - Google Patents
Procyanidine microcapsule and preparation method thereof Download PDFInfo
- Publication number
- CN114431466A CN114431466A CN202210098572.2A CN202210098572A CN114431466A CN 114431466 A CN114431466 A CN 114431466A CN 202210098572 A CN202210098572 A CN 202210098572A CN 114431466 A CN114431466 A CN 114431466A
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- procyanidin
- microcapsule
- distilled water
- mass ratio
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Links
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- XFZJEEAOWLFHDH-UHFFFAOYSA-N (2R,2'R,3R,3'R,4R)-3,3',4',5,7-Pentahydroxyflavan(48)-3,3',4',5,7-pentahydroxyflavan Natural products C=12OC(C=3C=C(O)C(O)=CC=3)C(O)CC2=C(O)C=C(O)C=1C(C1=C(O)C=C(O)C=C1O1)C(O)C1C1=CC=C(O)C(O)=C1 XFZJEEAOWLFHDH-UHFFFAOYSA-N 0.000 claims abstract description 143
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Images
Classifications
-
- 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
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
-
- 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
- A23L29/03—Organic compounds
- A23L29/035—Organic compounds containing oxygen as heteroatom
-
- 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
- A23L29/03—Organic compounds
- A23L29/045—Organic compounds containing nitrogen as heteroatom
-
- 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
- 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
- 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
Abstract
The invention discloses a proanthocyanidin microcapsule and a preparation method thereof. When the sodium alginate and the calcium form a calcium alginate capsule shell, the small molecular protein-whey protein is complexed with the procyanidine, so that the exudation of the procyanidine is reduced, and the stability of the procyanidine in the microcapsule is enhanced. Standing for a period of time, adding the microcapsule into the chitosan solution, and coating a layer of chitosan shell outside the existing microcapsule. And naturally drying to obtain the chitosan/calcium alginate/lactalbumin-procyanidine microcapsule. The microcapsule can obviously improve the stability of procyanidine. In addition, during simulated digestion, the procyanidin in the microcapsule is slowly released, the biological acceptable yield is high, and the chyme has little influence on the stability of the chyme.
Description
Technical Field
The invention relates to the technical field of improvement of procyanidine preparations, in particular to a procyanidine microcapsule and a preparation method thereof.
Background
Proanthocyanidin (PC), also called proanthocyanidin, refers to a polyphenol isolated from plants that produces anthocyanins (anthocyanidins) upon acidic hot alcohol treatment. Procyanidins include monomers and polymers, are widely distributed in nature and are found in a variety of plants and everyday foods. The monomeric procyanidin mainly comprises flavan-4-ol and flavan-3, 4-diol, while the polymeric procyanidin has two types of oligomerization and high polymerization. The multi-electron phenolic hydroxyl structure in the molecular structure of the procyanidin enables the procyanidin to have stronger physiological activity. Researches show that under the same conditions, the inhibition rate of the procyanidin on superoxide anions and hydroxyl radicals is 2 times that of vitamin E and 7 times that of vitamin C, and more than 80 diseases caused by free radicals can be prevented and treated. Meanwhile, procyanidine plays a certain role in the treatment and prevention of diseases such as tumors, cardiovascular and cerebrovascular diseases, inflammation, nervous system and the like, is widely used in the fields of health-care food, medicines, cosmetics and the like, and is a functional food raw material with great development prospect.
The existing oral procyanidin preparation is mostly a capsule or a soft capsule preparation, and is prepared by directly filling procyanidin powder into an empty capsule, adding other auxiliary materials into procyanidin to prepare uniform powder or granules, and then filling the uniform powder or granules into the empty capsule or mixing procyanidin and oil and fat and wrapping the mixture in a soft capsule shell. The procyanidin preparation has no sustained release effect, can be rapidly disintegrated in gastrointestinal tract after oral administration, and rapidly released, and is easily degraded and denatured under the alkaline condition of intestinal tract, thereby affecting bioavailability. In addition, procyanidin has active property, and phenolic hydroxyl, especially ortho-phenolic hydroxyl, is easy to be oxidized and denatured under the external environmental conditions of enzyme, air, moisture, high pH and the like, and is also easy to react with metal ions, food additives and other components, so that the stability is reduced.
The procyanidin has the following problems in specific use:
1. procyanidins are poorly stable and easily degradable. High temperature, light, alkaline environment, partial metal ions and food additives all affect the stability of the food, so that the food loses the antioxidant activity. Under the condition of partial alkalinity (pH8.0), the content of the procyanidine of the lycium ruthenicum mill which is stored in a sealed and sealed mode at room temperature is only 20% of the initial content after being stored for 3 days, and the content of the procyanidine of the lycium ruthenicum mill which is stored for 36 hours at 50 ℃ is only 60% of the initial content. Li and other grape seed procyanidin are dissolved in buffer solution, sealed and kept stand for 12 hours, the content of the grape seed procyanidin in the solution with the pH value of 6.0 is reduced to 38.8 percent, the content of the grape seed procyanidin in the solution with the pH value of 3.0 is only 42 percent, and common Al is added3+、Zn2+、Na+、Mg2+、Fe2+The ions all have great influence on the stability of the procyanidin. The instability of the property of the procyanidin makes the procyanidin be easily damaged by oxidation during the storage, transportation and use processes, and the application condition and range are greatly limited.
2. The biological acceptability of procyanidins is low. When proanthocyanidins are ingested by a human body, complex chyme components in the gastrointestinal tract also react with the proanthocyanidins to change the existing configuration and absorption of the proanthocyanidins, so that the proanthocyanidins are ineffective. Therefore, the antioxidant activity of procyanidin in vitro experiments is well verified in the existing research, but the effectiveness of procyanidin in animal or human body experiments is not obvious once the procyanidin is used in the animal or human body experiments.
3. Procyanidins have strong astringent taste, and the addition of procyanidins to foods can significantly affect the mouthfeel. Procyanidin is one of plant polyphenols, and can react with oral cell surface protein to strongly influence the taste of food containing procyanidin. Meanwhile, the procyanidin powder is reddish brown to tan, and the color of the food can be changed after the procyanidin powder is added into the food. The characteristics of procyanidins influence the further application of procyanidins in the fields of foods and functional foods.
For example, the application number is [ CN201910881304.6 ] a preparation method of a gelatin-sodium alginate complex coacervate procyanidin microcapsule, belonging to the technical field of microcapsule preparation. The method comprises the steps of taking procyanidin as a raw material, uniformly mixing an aqueous solution of procyanidin with a gelatin solution, adding a sodium alginate solution, adjusting the pH value of the solution to enable gelatin and sodium alginate to generate complex coacervation reaction through electrostatic interaction, adding a salt solution containing divalent calcium ions as a cross-linking agent to form complex coacervate, depositing the complex coacervate around procyanidin to form a microcapsule, centrifuging, freezing and drying to obtain the gelatin-sodium alginate complex coacervate procyanidin microcapsule, wherein the microcapsule can obviously improve the stability of procyanidin, provides a research basis for modifying complex polymers induced by calcium ions, particularly gelatin, and can provide a new thought for developing complex carriers with biological activity, and has an important effect on promoting the practical application of complex coacervate microcapsules in the field of foods.
However, the gelatin in the gelatin-sodium alginate complex coacervation procyanidin microcapsule prepared by the method belongs to macromolecular protein and is difficult to digest in the gastrointestinal tract of a human body, and the absorption and utilization of the coated procyanidin in the gastrointestinal tract are influenced. Meanwhile, the macromolecular gelatin has a certain cross-linking characteristic, the coating rate of the macromolecular gelatin to the procyanidine is low during the preparation, when a human body takes the microcapsule, the uncoated procyanidine can be quickly released at the front end of the digestive tract to react with complex chyme components in the gastrointestinal tract, the existing configuration and absorption of the procyanidine are changed, and the procyanidine is caused to lose efficacy.
The microcapsule technology is a high-new deep processing technology which is popular in the fields of food, agricultural products, pharmacy and the like in recent years. It refers to a technique of wrapping particles, liquid drops or bubbles (generally called as core materials) into heterogeneous particles by using high molecular materials (generally called as wall materials), and has the advantages of protecting the physical state of the materials in the capsule, isolating active ingredients, enhancing the processing performance and the like. In the preparation of microcapsules, the selection of wall materials is very important. Some documents have been used to study the preparation process of procyanidin microcapsules. Fabri cio l, Tulini, etc. cinnamon procyanidin microcapsules were prepared using hydrogenated soybean oil, cottonseed oil, and palm oil; embedding procyanidine with acacia and beta-cyclodextrin; wang et al prepared grape polyphenol microcapsules using an ethanol solution of acrylic resin S100 as a coating solution. However, these studies have problems that the wall material is not healthy enough, the microcapsule encapsulation performance is poor (the improvement of the procyanidin stability is not significant), the digestive tract disintegration rate is not high, and the bioavailability is poor.
The search for safe and efficient natural antioxidants from plant resources has been the focus and attention of many researchers. Although China has rich plant resources, the development of deep processing of food is always slow, and many high-quality food raw materials have the problems of poor stability and the like, so that the international market lacks competitiveness. Under the premise, if a procyanidin microcapsule can be developed, the stability of procyanidin can be improved in storage, the slow release property of procyanidin can be kept in the digestion process, and the procyanidin and macromolecules in chyme are prevented from being subjected to complex precipitation, so that the absorption is influenced, and the application effect of procyanidin in foods and functional foods can be obviously improved.
Disclosure of Invention
In order to solve the problems, the invention provides the procyanidine microcapsule and the preparation method thereof, which complex micromolecule protein-whey protein with procyanidine, can improve the stability of procyanidine in storage, can keep the slow release characteristic of procyanidine in the digestion process, and prevents the procyanidine from being complexed and precipitated with macromolecules in chyme.
In order to achieve the purpose, the invention is realized by the following technical scheme: in one aspect, the invention provides a preparation method of procyanidine microcapsules, which comprises the following steps:
s1, removing impurities, dissolving procyanidin, mixing procyanidin, ethanol and water to obtain procyanidin solution, and placing in a dark place for use;
s2, dissolving sodium alginate in distilled water to obtain a sodium alginate solution;
s3, mixing the procyanidin solution in the S1 and the sodium alginate solution in the S2 according to the mass ratio of 1:1, and dispersing to obtain a solution A;
s4, dissolving chitosan in distilled water to obtain a chitosan solution;
s5, dissolving the whey protein in distilled water, and heating for denaturation to obtain a whey protein solution;
s6, dissolving calcium lactate in distilled water to obtain a calcium lactate solution, mixing the whey protein solution and the calcium lactate solution in the S5 according to the mass ratio of 1:1, and uniformly mixing to form a solution B;
s7, sucking the solution A in the S3 into an injector, installing a needle, dripping the solution A10-15 cm above the solution B in the S6 at a constant speed, reacting for 10-100min to form a microcapsule, filtering, transferring the microcapsule into a chitosan solution in the S4 to obtain a wet capsule, washing, filtering and airing to obtain the procyanidine microcapsule.
In the present invention, the longer the reaction time is after dropping the solution a into the solution B, the thicker the capsule shell of the microcapsule is formed. The microcapsule can be formed within 10-100 min.
Preferably, the mass ratio of procyanidine, ethanol and water in the S1 is (10-12): (2-7): (27-48).
In the invention, the procyanidine has different qualities, and the required ethanol amount and water amount are different. According to the experimental results, the content of the oligomer is high, the solubility is good, the content of the oligomer is low, and the solubility is poor.
Preferably, the mass ratio of the sodium alginate to the distilled water in the S2 is (2-4): 90.
preferably, the mass ratio of chitosan to distilled water in S4 is 1: 50.
preferably, the mass ratio of the whey protein to the distilled water in the S5 is (0.1-1): 50.
preferably, the heat denaturation conditions in S5 are as follows: heating in water at 85-100 deg.C for 10 min.
In the present invention, the purpose of the water bath is to denature the whey protein and to unfold the folding structure of the whey protein.
Preferably, the mass ratio of calcium lactate to distilled water in S6 is 1: 10.
on the other hand, the invention also provides the procyanidine microcapsule prepared by the method.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a proanthocyanidin microcapsule, which takes proanthocyanidin as a raw material, mixes the solution of the proanthocyanidin with a sodium alginate solution, and drips the mixed solution into a mixed solution of calcium lactate and lactalbumin with a certain concentration. When the sodium alginate and the calcium form a calcium alginate capsule shell, the small molecular protein-whey protein is complexed with the procyanidine, so that the exudation of the procyanidine is reduced, and the stability of the procyanidine in the microcapsule is enhanced. Standing for a period of time, adding the microcapsule into the chitosan solution, and coating a layer of chitosan shell outside the existing microcapsule. Then naturally drying to obtain the chitosan/calcium alginate/whey protein-procyanidin microcapsule. The microcapsule can obviously improve the stability of procyanidine. In addition, during simulated digestion, the procyanidin in the microcapsule is slowly released, the biological acceptable yield is high, and the chyme has little influence on the stability of the chyme.
Drawings
Fig. 1 is a flow chart of a method for preparing procyanidin microcapsules according to an embodiment of the invention.
FIG. 2 is a diagram showing the behavior of microcapsules according to the present invention.
FIG. 3 is a line graph of the retention rates of three microcapsules and procyanidin powder at 100 ℃ in the examples of the present invention.
FIG. 4 is a bar graph of the retention of three microcapsules and procyanidin powder under light in the examples of the invention.
Fig. 5 is a bar graph of the release rates of three microcapsules and procyanidin powder in simulated digestion according to the examples of the invention.
FIG. 6 is a line graph showing the release rates of the three microcapsules and the procyanidin powder at the whole digestion stage in the examples of the present invention.
Detailed Description
In order to more clearly illustrate the embodiments of the present invention and the technical solutions in the prior art, the following will describe the specific embodiments of the present invention with reference to the accompanying drawings.
It is obvious that the drawings in the following description are only some examples of the invention, and it is obvious to a person skilled in the art that other drawings and other embodiments can be obtained from these drawings without inventive effort, and the invention is not limited to this example.
The specific embodiment of the invention is as follows:
example 1
A procyanidin microcapsule comprises whey protein complex and procyanidin complex, calcium alginate capsule shell on the outer layer of the complex, and chitosan shell on the outer layer of the calcium alginate capsule shell.
In this example:
a method for preparing procyanidin microcapsule comprises:
s1, removing impurities, dissolving procyanidin, mixing procyanidin, ethanol and water to obtain procyanidin solution, and placing in a dark place for use; the mass ratio of the procyanidine to the ethanol to the water is 10: 2: 27;
s2, dissolving sodium alginate in distilled water to obtain a sodium alginate solution; the mass ratio of the sodium alginate to the distilled water is 2: 90, respectively;
s3, mixing the procyanidin solution in the S1 and the sodium alginate solution in the S2 according to the mass ratio of 1:1, and dispersing to obtain a solution A;
s4, dissolving chitosan in distilled water to obtain a chitosan solution; the mass ratio of the chitosan to the distilled water is 1: 50;
s5, dissolving the whey protein in distilled water, and heating until the whey protein is denatured to obtain a whey protein solution; the mass ratio of the whey protein to the distilled water is 0.1: 50; the heating conditions were: heating in water at 85 deg.C for 10 min;
s6, dissolving calcium lactate in distilled water to obtain a calcium lactate solution, mixing the whey protein solution and the calcium lactate solution in the S5 according to a mass ratio of 1:1 to ensure that the final concentration of the whey protein is 2% (the concentration of the whey protein can be changed to a certain extent, and the whey protein solution needs to be heated or boiled in a water bath to be fully denatured and is structurally opened), and uniformly mixing to form a solution B; the mass ratio of calcium lactate to distilled water is 1: 10;
s7, sucking the solution A in the S3 into an injector, installing a needle, dripping the solution A10 cm above the solution B in the S6 at a constant speed, reacting for 10min to form a microcapsule, transferring the microcapsule into a chitosan solution in the S4 to obtain a wet capsule, washing, filtering and airing to obtain the procyanidin microcapsule.
Example 2
A procyanidin microcapsule comprises whey protein complex and procyanidin complex, calcium alginate capsule shell on the outer layer of the complex, and chitosan shell on the outer layer of the calcium alginate capsule shell.
In this example:
a method for preparing procyanidin microcapsule comprises:
s1, removing impurities, dissolving procyanidin, mixing procyanidin, ethanol and water to obtain procyanidin solution, and placing in a dark place for use; the mass ratio of the procyanidine to the ethanol to the water is 11: 5: 37;
s2, dissolving sodium alginate in distilled water to obtain a sodium alginate solution; the mass ratio of the sodium alginate to the distilled water is 3: 90, respectively;
s3, mixing the procyanidin solution in the S1 and the sodium alginate solution in the S2 according to the mass ratio of 1:1, and dispersing to obtain a solution A;
s4, dissolving chitosan in distilled water to obtain a chitosan solution; the mass ratio of the chitosan to the distilled water is 1: 50;
s5, dissolving whey protein in distilled water, and heating until the whey protein is denatured to obtain whey protein solution; the mass ratio of the whey protein to the distilled water is 0.5: 50; the heating conditions were: heating in 93 deg.C water for 10 min;
s6, dissolving calcium lactate in distilled water to obtain a calcium lactate solution, mixing the whey protein solution and the calcium lactate solution in the S5 according to a mass ratio of 1:1 to ensure that the final concentration of the whey protein is 2% (the concentration of the whey protein can be changed to a certain extent, and the whey protein solution needs to be heated or boiled in a water bath to be fully denatured and is structurally opened), and uniformly mixing to form a solution B; the mass ratio of calcium lactate to distilled water is 1: 10;
s7, sucking the solution A in the S3 into an injector, installing a needle, dripping the solution A13 cm above the solution B in the S6 at a constant speed, reacting for 50min to form a microcapsule, transferring the microcapsule into a chitosan solution in the S4 to obtain a wet capsule, washing, filtering and airing to obtain the procyanidin microcapsule.
Example 3
A procyanidin microcapsule comprises complex of whey protein and procyanidin, calcium alginate shell on the outer layer of the complex, and chitosan shell on the outer layer of the calcium alginate shell.
In this example:
a method for preparing procyanidin microcapsule comprises:
s1, removing impurities, dissolving procyanidin, mixing procyanidin, ethanol and water to obtain procyanidin solution, and placing in a dark place for use; the mass ratio of the procyanidine to the ethanol to the water is 12: 7: 48;
s2, dissolving sodium alginate in distilled water to obtain a sodium alginate solution; the mass ratio of the sodium alginate to the distilled water is 4: 90, respectively;
s3, mixing the procyanidin solution in the S1 and the sodium alginate solution in the S2 according to the mass ratio of 1:1, and dispersing to obtain a solution A;
s4, dissolving chitosan in distilled water to obtain a chitosan solution; the mass ratio of the chitosan to the distilled water is 1: 50;
s5, dissolving the whey protein in distilled water, and heating until the whey protein is denatured to obtain a whey protein solution; the mass ratio of the whey protein to the distilled water is 1: 50; the heating conditions were: heating in 100 deg.C water for 10 min;
s6, dissolving calcium lactate in distilled water to obtain a calcium lactate solution, mixing the whey protein solution and the calcium lactate solution in the S5 according to a mass ratio of 1:1 to ensure that the final concentration of the whey protein is 2% (the concentration of the whey protein can be changed to a certain extent, and the whey protein solution needs to be heated or boiled in a water bath to be fully denatured and is structurally opened), and uniformly mixing to form a solution B; the mass ratio of calcium lactate to distilled water is 1: 10;
s7, sucking the solution A in the S3 into an injector, installing a needle, dripping the solution A15 cm above the solution B in the S6 at a constant speed, reacting for 100min to form a microcapsule, transferring the microcapsule into a chitosan solution in the S4 to obtain a wet capsule, washing, filtering and airing to obtain the procyanidin microcapsule.
Comparative example 1
A microcapsule containing calcium alginate procyanidin comprises procyanidin and calcium alginate capsule shell on the outer layer of procyanidin.
In this comparative example:
a method for preparing calcium alginate procyanidin microcapsule comprises:
s1, removing impurities, dissolving procyanidin, fully and uniformly mixing procyanidin, ethanol and water to obtain procyanidin solution, and placing in a dark place for later use; the mass ratio of procyanidine to ethanol to water is 11: 5: 37;
s2, dissolving sodium alginate in distilled water to obtain a sodium alginate solution; the mass ratio of the sodium alginate to the distilled water is 3: 90, respectively;
s3, mixing the procyanidin solution in the S1 and the sodium alginate solution in the S2 according to the mass ratio of 1:1, and dispersing to obtain a solution A;
s4, dissolving calcium lactate in distilled water to obtain a calcium lactate solution; the mass ratio of calcium lactate to distilled water is 1: 10;
s5, sucking the solution A in the S3 into an injector, installing a needle, dripping 13cm above the calcium lactate solution in the S4 at a constant speed, reacting for 50min to form a microcapsule, washing, filtering and airing to obtain the calcium alginate procyanidin microcapsule.
Comparative example 2
A whey protein-calcium alginate procyanidin microcapsule comprises complex of whey protein and procyanidin, and calcium alginate capsule shell on the outer layer of procyanidin.
In this comparative example:
a method for preparing lactalbumin-calcium alginate procyanidin microcapsule comprises:
s1, removing impurities, dissolving procyanidin, mixing procyanidin, ethanol and water to obtain procyanidin solution, and placing in a dark place for use; the mass ratio of procyanidine to ethanol to water is 11: 5: 37;
s2, dissolving sodium alginate in distilled water to obtain a sodium alginate solution; the mass ratio of the sodium alginate to the distilled water is 3: 90;
s3, mixing the procyanidin solution in the S1 and the sodium alginate solution in the S2 according to the mass ratio of 1:1, and dispersing to obtain a solution A;
s4, dissolving the whey protein in distilled water, and heating until the whey protein is denatured to obtain a whey protein solution; the mass ratio of the whey protein to the distilled water is 0.5: 50; the conditions for heat denaturation were: heating in 93 deg.C water for 10 min;
s5, dissolving calcium lactate in distilled water to obtain a calcium lactate solution, mixing the whey protein solution and the calcium lactate solution in the S4 according to the mass ratio of 1:1, and uniformly mixing to form a solution B; the mass ratio of calcium lactate to distilled water is 1: 10;
s6, sucking the solution A in S3 into an injector, installing a needle, dripping the solution A13 cm above the solution B in S5 at a constant speed, reacting for 50min to form a microcapsule, washing, filtering and airing to obtain the whey protein-calcium alginate procyanidin microcapsule.
Comparative example 3
A gelatin-calcium alginate procyanidin microcapsule comprises complex of gelatin and procyanidin, and calcium alginate capsule shell located on outer layer of procyanidin. This comparative example 3 is different from comparative example 2 in that gelatin-calcium alginate procyanidin microcapsules are prepared by replacing whey protein with gelatin.
Comparative example 4
A chitosan-gelatin-calcium alginate microcapsule comprises a complex of gelatin and procyanidin, a calcium alginate capsule shell positioned on the outer layer of procyanidin, and a chitosan shell positioned on the outer layer of the calcium alginate capsule shell.
In this comparative example:
a preparation method of chitosan-gelatin-calcium alginate microcapsules comprises the following steps:
s1, removing impurities, dissolving procyanidin, mixing procyanidin, ethanol and water to obtain procyanidin solution, and placing in a dark place for use; the mass ratio of the procyanidine to the ethanol to the water is 11: 5: 37;
s2, dissolving sodium alginate in distilled water to obtain a sodium alginate solution; the mass ratio of the sodium alginate to the distilled water is 3: 90, respectively;
s3, mixing the procyanidin solution in the S1 and the sodium alginate solution in the S2 according to the mass ratio of 1:1, and dispersing to obtain a solution A;
s4, dissolving chitosan in distilled water to obtain a chitosan solution; the mass ratio of the chitosan to the distilled water is 1: 50;
s5, dissolving gelatin in distilled water, and heating to obtain gelatin solution; the mass ratio of the gelatin to the distilled water is 0.5: 50; the heating conditions were: heating in 93 deg.C water for 10 min;
s6, dissolving calcium lactate in distilled water to obtain a calcium lactate solution, mixing the gelatin solution and the calcium lactate solution in the S5 according to the mass ratio of 1:1, and uniformly mixing to form a solution B; the mass ratio of calcium lactate to distilled water is 1: 10;
s7, sucking the solution A in the S3 into an injector, installing a needle, dripping the solution A13 cm above the solution B in the S6 at a constant speed, reacting for 50min to form a microcapsule, transferring the microcapsule into a chitosan solution in the S4 to obtain a wet capsule, washing, filtering and airing to obtain the chitosan-gelatin-calcium alginate microcapsule.
Comparative example 5
A chitosan-calcium alginate microcapsule comprises procyanidin, calcium alginate capsule shell located on the outer layer of procyanidin, and chitosan shell located on the outer layer of calcium alginate capsule shell.
In this comparative example:
a preparation method of chitosan-calcium alginate microcapsules comprises the following steps:
s1, removing impurities, dissolving procyanidin, mixing procyanidin, ethanol and water to obtain procyanidin solution, and placing in a dark place for use; the mass ratio of the procyanidine to the ethanol to the water is 11: 5: 37;
s2, dissolving sodium alginate in distilled water to obtain a sodium alginate solution; the mass ratio of the sodium alginate to the distilled water is 3: 90;
s3, mixing the procyanidin solution in the S1 and the sodium alginate solution in the S2 according to the mass ratio of 1:1, and dispersing to obtain a solution A;
s4, dissolving chitosan in distilled water to obtain a chitosan solution; the mass ratio of the chitosan to the distilled water is 1: 50;
s5, dissolving calcium lactate in distilled water to obtain a calcium lactate solution; the mass ratio of calcium lactate to distilled water is 1: 10;
s6, sucking the solution A in the S3 into an injector, installing a needle, dripping 13cm above the calcium lactate solution in the S5 at a constant speed, reacting for 50min to form a microcapsule, transferring the microcapsule into the chitosan solution in the S4 to obtain a wet capsule, washing, filtering and airing to obtain the chitosan-calcium alginate microcapsule.
The microcapsules prepared in example 2 and comparative examples 1-5 were named as shown in table 1.
TABLE 1 sample name and corresponding Capsule name
| Test specimen | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 | Example 2 |
| Name of capsule | Capsule A | Capsule B | Capsule C | Capsule D | Capsule E | Capsule F |
The capsules a-F were tested:
microcapsule character test:
the microcapsules prepared in example 2 and comparative examples 1 to 5 were observed by an electron microscope, and the results are shown in fig. 2. According to the performance of the dried microcapsule, it can be found that when different molecular wall materials are selected, some wall materials can be directly wrapped to form the microcapsule with better property, and some wall materials cannot form the microcapsule with good property due to the weak cross-linking reaction between macromolecules and the influence of the property of polyphenol functional components.
From the preliminary screening, it can be seen from fig. 2 that the microcapsules prepared in comparative example 1, comparative example 5 and example 2 have relatively good properties. Capsule A, capsule E and capsule F. And the three microcapsules were selected for subsequent testing.
Thermal stability test:
the three microcapsules were heated in a water bath at 100 ℃. Using a colorimetric tube, weighing three capsules and procyanidine powder respectively, adding a proper amount of potassium dihydrogen phosphate buffer solution with the pH value of 6.0, then putting the capsules and procyanidine powder into a water bath kettle for water bath heating, heating in the water bath for 0min, 15 min, 30 min, 60 min, 90 min, 120 min, 180 min and 240 min, taking out a group of colorimetric tubes each time, cooling the colorimetric tubes by cold water for 10min, homogenizing, completely destroying microcapsules, absorbing the solution, diluting to a certain degree, measuring the content of procyanidine, and performing three parallel experiments. The results are shown in Table 2. And the results of table 2 were made into a linear graph as shown in fig. 3.
Table 2: storage rate of three kinds of microcapsules and procyanidin powder at 100 ℃ (n = 3)
As can be seen from table 2, microencapsulation can significantly improve the thermal stability of procyanidins. After 4 or more hours of tests, the procyanidin powder loses about 50% even under slightly acidic conditions, and the loss of the three microcapsules is about 20-30%. The chitosan-whey protein-calcium alginate procyanidin microcapsule (capsule F) prepared in example 2 has the highest thermal stability, and only 20.3% of the microcapsule is lost after being heated for 4 hours or more at 100 ℃, which is obviously lower than the microcapsule prepared by other wall materials. The calcium alginate procyanidin microcapsule (capsule A) and the chitosan-calcium alginate microcapsule (capsule E) are different from the assumption that the thermal stability of the capsule A is higher than that of the capsule E. By analyzing the properties of the wall material, the chitosan is food polysaccharide with negative charges and is alkaline in the microenvironment of the system. Procyanidins are stable under acidic conditions and are easily decomposed under alkaline conditions. During storage, the alkalinity of chitosan itself in a microenvironment affects the core material in the microcapsules, thereby reducing the stability of procyanidins. While the alkalinity in the microenvironment reduces the effect on the stability of the procyanidins when it is complexed with whey proteins, thereby maximizing the stability of the capsule F.
And (3) light stability test:
irradiating the three capsules A, E and F and the procyanidin powder for 20 hours under illumination, soaking the capsules in a buffer solution with the pH value of 6.0 for 1 hour, homogenizing, releasing the procyanidin in the microcapsules, and determining the content of the procyanidin by constant volume absorption solution. The measurement results are shown in table 3. And the results of table 3 were made into a bar graph as shown in fig. 4.
Table 3: preservation of three microcapsules and procyanidin powder after light exposure (n = 3)
| Time of heating | Storage ratio (%) | SD |
| Capsule A | 77.3 | 4.1 |
| Capsule E | 76.8 | 9.3 |
| Capsule F | 85.5 | 7.1 |
| Powder of | 62.5 | 3.8 |
As is clear from the results in table 3, microencapsulation significantly improved the photostability of procyanidins. After illumination, the preservation rate of the procyanidin powder is only 62.5 +/-3.8 percent of the original preservation rate, while the preservation rate of the capsule A is 77.3 +/-4.1 percent, the preservation rate of the capsule E is 76.8 +/-9.3 percent, and the preservation rate of the capsule F with the strongest stability is 85.5 +/-7.1 percent. The photostability test shows that in the capsule F, whey protein was used to complex procyanidin, thereby significantly increasing the photostability of procyanidin.
Biological acceptability test in simulated digestion process:
a static continuous in-vitro digestion system is established to respectively simulate the digestion of the oral cavity, the stomach and the intestinal tract of a human body. Digesting the three capsules of the capsule A, the capsule E and the capsule F and the procyanidin powder in a digestive system for a period of time, and analyzing the content of procyanidin released into digestive juice. The results are shown in Table 4. And the results of table 4 were made into bar graphs and linear graphs as shown in fig. 5 and 6.
Table 4: release rate of three microcapsules and powder in simulated digestion process (n = 3)
As can be seen from the results shown in table 4, fig. 5, and fig. 6, the release rate of the microencapsulated procyanidins was low and the release rate of the powder was very high in the oral phase. However, in the stomach stage, procyanidin powder can combine with digestive enzymes in the stomach to form complex, and the release rate is reduced rapidly. At this time, the procyanidin in the three microcapsules still enters the digestive juice in a slow release mode. When the digestion stage enters the intestine, the proanthocyanidin release rate of the powder sample increases first due to the action of the protease, but gradually decreases due to the instability of the proanthocyanidin under the alkaline condition. The biologically acceptable yield of procyanidins in the powder in the intestinal tract is approximately 26.2% + -6.7% according to the calculation method of the biologically acceptable yield. The three microcapsules wrap the procyanidin in the capsule shell, so that the procyanidin is slowly released all the time in the early and middle stages of the digestion process, the microenvironment concentration of the procyanidin is reduced, and the probability of generating a complex compound with protein in a digestive juice is reduced. Therefore, when the three microcapsules are digested in a simulated mode, the procyanidine is released continuously and slowly, and the biological acceptability is higher than that of powder.
In addition, among the three microcapsules, the capsule F prepared in this example 2 has a low release rate in the oral cavity and the stomach, and after entering the intestinal tract, the release rate gradually increases under the action of intestinal protease, and after intestinal digestion for 2 hours, the bioacceptable rate of the capsule a is 46.9% ± 1.4%, the biological acceptability of the capsule E is 60.7% ± 7.1%, and the biological acceptability of the capsule F is 60.9% ± 2.1%, which indicates that the intestinal acceptability of the capsules E and F in the absorption part is high.
Compared with the capsule E, the capsule F releases more slowly in the early stage, which is beneficial to storing procyanidine, and the capsule E is added to the capsule F in the later stage of the intestinal part, which promotes the absorption of the microcapsule in the intestinal tract, and shows that the biological acceptability of the capsule F is higher. The microcapsule can obviously improve the absorption problem of procyanidine, and the coating process of the capsule F has a promoting effect on the absorption of the microcapsule in intestinal tracts.
Test of improving effect on mouthfeel:
selecting brewed lotus root starch, respectively adding a certain amount of procyanidine powder and three kinds of microcapsules, and uniformly stirring. According to the scoring criteria in table 6, 30 subjects (age 19-50, 13 men and 17 women) were asked to score their tastes and compare them with the original lotus root starch. The results are shown in tables 5 and 6.
TABLE 5 sensory evaluation Table
| Item | Evaluation criteria |
| Sour taste | Obvious sourness is 1 point; the sourness is general and can be accepted for 3 points; no sour taste 5 points |
| Bitter taste | Has obvious bitter taste of 1 point; the sourness is general and can be accepted for 3 points; no sour taste 5 points |
| Astringent taste | Obvious astringent taste of 1 point; the sourness is general and can be accepted for 3 points; no sour taste 5 points |
| Overall mouthfeel | The overall taste is poor by 1 point; the mouthfeel is changed, but 3 points can be accepted; no mouth feel change 5 points |
Table 6 sensory evaluation results (n = 30)
| Item | Sour taste | Bitter taste | Astringent taste | Overall mouthfeel | Sum of scores |
| Capsule A | 4 | 4 | 4 | 4 | 16 |
| Capsule E | 5 | 5 | 5 | 5 | 20 |
| Capsule F | 5 | 5 | 5 | 5 | 20 |
| Powder of | 3 | 1.5 | 1 | 1 | 6.5 |
From the results in tables 5 to 6, it is understood that microencapsulation can shield the bitterness and astringency of the procyanidin powder, improve the mouthfeel of the procyanidin added to food, and increase the possibility of its application in food. Meanwhile, in the three microcapsules, the capsule E, F has 2-3 layers of capsule shell structures in embedding, so that the release of the microcapsules in food is reduced, and the effect of improving the mouthfeel is the best.
Therefore, the procyanidin in the microcapsule prepared by the embodiment has high stability, is slowly released in a digestive system, has high biologically acceptable yield, and has little influence of chyme on the stability and high nutritional value.
The above-described aspects may be implemented individually or in various combinations, and such variations are within the scope of the present invention.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the specific embodiments of the invention be limited to these descriptions. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.
Claims (8)
1. A preparation method of procyanidine microcapsules is characterized by comprising the following steps:
s1, removing impurities, dissolving procyanidin, fully and uniformly mixing procyanidin, ethanol and water to obtain procyanidin solution, and placing in a dark place for later use;
s2, dissolving sodium alginate in distilled water to obtain a sodium alginate solution;
s3, mixing the procyanidin solution in the S1 and the sodium alginate solution in the S2 according to the mass ratio of 1:1, and dispersing to obtain a solution A;
s4, dissolving chitosan in distilled water to obtain a chitosan solution;
s5, dissolving the whey protein in distilled water, and heating for denaturation to obtain a whey protein solution;
s6, dissolving calcium lactate in distilled water to obtain a calcium lactate solution, mixing the whey protein solution and the calcium lactate solution in the S5 according to the mass ratio of 1:1, and uniformly mixing to form a solution B;
s7, sucking the solution A in the S3 into an injector, installing a needle, dripping the solution A10-15 cm above the solution B in the S6 at a constant speed, reacting for 10-100min to form a microcapsule, filtering, transferring the microcapsule into a chitosan solution in the S4 to obtain a wet capsule, washing, filtering and airing to obtain the procyanidine microcapsule.
2. The method for preparing procyanidin microcapsules according to claim 1, wherein the mass ratio of procyanidin, ethanol and water in the S1 is (10-12): (2-7): (27-48).
3. The method for preparing procyanidin microcapsules according to claim 1, wherein the mass ratio of sodium alginate to distilled water in S2 is (2-4): 90.
4. the method for preparing procyanidin microcapsules according to claim 1, wherein a mass ratio of chitosan to distilled water in S4 is 1: 50.
5. the method for preparing procyanidin microcapsules according to claim 1, wherein the mass ratio of whey protein to distilled water in S5 is (0.1-1): 50.
6. the method for preparing procyanidin microcapsules according to claim 1, wherein the heat denaturation in the S5 is performed under the following conditions: heating in water at 85-100 deg.C for 10 min.
7. The method for preparing procyanidin microcapsules according to claim 1, wherein the mass ratio of calcium lactate to distilled water in S6 is 1: 10.
8. a procyanidin microcapsule obtainable by the method of preparation as claimed in claims 1 to 7.
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| CN114870758A (en) * | 2022-05-11 | 2022-08-09 | 杭州职业技术学院 | Device for continuously producing microcapsules and using method thereof |
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