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CN114831957A - Diglyceride microcapsule prepared by using Maillard reaction product and preparation method thereof - Google Patents

Diglyceride microcapsule prepared by using Maillard reaction product and preparation method thereof Download PDF

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Publication number
CN114831957A
CN114831957A CN202210451974.6A CN202210451974A CN114831957A CN 114831957 A CN114831957 A CN 114831957A CN 202210451974 A CN202210451974 A CN 202210451974A CN 114831957 A CN114831957 A CN 114831957A
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diglyceride
wall material
microcapsules
whey protein
protein isolate
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CN114831957B (en
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王祝彬
李进伟
涂静
江运秋
黄生权
郭凌溪
欧成成
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Npgs Guangdong Biotechnology Co ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/48Preparations in capsules, e.g. of gelatin, of chocolate
    • A61K9/50Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
    • A61K9/5005Wall or coating material
    • A61K9/5021Organic macromolecular compounds
    • A61K9/5052Proteins, e.g. albumin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00Medicinal preparations containing organic active ingredients
    • A61K31/21Esters, e.g. nitroglycerine, selenocyanates
    • A61K31/215Esters, e.g. nitroglycerine, selenocyanates of carboxylic acids
    • A61K31/22Esters, e.g. nitroglycerine, selenocyanates of carboxylic acids of acyclic acids, e.g. pravastatin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/48Preparations in capsules, e.g. of gelatin, of chocolate
    • A61K9/50Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
    • A61K9/5005Wall or coating material
    • A61K9/5021Organic macromolecular compounds
    • A61K9/5036Polysaccharides, e.g. gums, alginate; Cyclodextrin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P13/00Drugs for disorders of the urinary system
    • A61P13/12Drugs for disorders of the urinary system of the kidneys
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P3/00Drugs for disorders of the metabolism
    • A61P3/04Anorexiants; Antiobesity agents
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P3/00Drugs for disorders of the metabolism
    • A61P3/06Antihyperlipidemics
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P3/00Drugs for disorders of the metabolism
    • A61P3/08Drugs for disorders of the metabolism for glucose homeostasis
    • A61P3/10Drugs for disorders of the metabolism for glucose homeostasis for hyperglycaemia, e.g. antidiabetics

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  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • General Chemical & Material Sciences (AREA)
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  • Obesity (AREA)
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  • Urology & Nephrology (AREA)
  • Manufacturing Of Micro-Capsules (AREA)

Abstract

The invention discloses a diglyceride microcapsule prepared by using Maillard reaction products and a preparation method thereof. The method comprises the following steps: mixing wall material formed by mixing whey protein isolate, sodium caseinate, sodium starch octenyl succinate and polydextrose with diglyceride oil, and homogenizing the obtained mixture under high pressure to obtain diglyceride microcapsules; wherein the whey protein isolate, the sodium caseinate, the sodium starch octenyl succinate and the polydextrose are in a mass part ratio of (3-6): (0.5-2): (1-3): (7-9), wherein the pH value of the wall material is 7-8. According to the diglyceride microcapsule disclosed by the invention, the stability of an emulsion formed by mixing the wall material and the core material is improved through the synergistic action of all components in the wall material and the synergistic action between the wall material and the core material, and the embedding rate and the storage stability of the prepared diglyceride microcapsule are greatly improved.

Description

Diglyceride microcapsule prepared by using Maillard reaction product and preparation method thereof
Technical Field
The invention belongs to the technical field of grease microcapsules, and particularly relates to a diglyceride microcapsule prepared by using Maillard reaction products and a preparation method thereof.
Background
Diglyceride oil is a functional oil and fat, and is a product obtained by esterification reaction of two hydroxyl groups in glycerol and fatty acid. In recent years, studies have found that diglyceride oil has effects of reducing accumulation of visceral fat, controlling body weight, improving blood lipid level, preventing arterial thrombosis, alleviating diabetes and nephropathy, and the like, and thus has received much attention. The unique metabolic profile of diglyceride oils is believed to be responsible for their particular physiological functions. The decomposition products of diglyceride oil after entering human body are 1-monoglyceride and free fatty acid, and the 1-monoglyceride and free fatty acid can not be esterified to triglyceride by 2-monoglyceride route, thereby reducing accumulation of triglyceride. In addition, the ingestion of the diglyceride oil promotes the improvement of the activity of enzymes related to beta oxidation, and can promote the decomposition of free fatty acids, thereby reducing the re-synthesis of triglyceride in vivo, reducing triglyceride in blood circulation, and playing roles in reducing blood lipid level and fat accumulation.
However, liquid diglyceride oils have the disadvantages of poor stability, poor solubility in water, low oral availability, etc., which limits the usefulness of the diglyceride oils in food products. To overcome these disadvantages, encapsulation of functional oils into emulsion-based microcapsule systems is a potential approach. The microcapsule can pulverize the liquid diglyceride oil, can maintain the original characteristics, performances and biological activity of the diglyceride oil to the maximum extent through morphological change and active substance release regulation, can effectively prevent the oxidation of the diglyceride oil and the volatilization of flavor substances, and effectively avoids the reaction of the diglyceride oil with the external environment, thereby effectively preventing the damage and loss of nutrient substances in the diglyceride oil. Therefore, the search for a wall material suitable for the diglyceride oil has important research significance, and is beneficial to widening the application field of the diglyceride oil.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art described above. Therefore, the invention provides a diglyceride microcapsule prepared by using Maillard reaction products and a preparation method thereof. The core material is diglyceride oil, the wall material is prepared from whey protein isolate, sodium caseinate, sodium starch octenyl succinate and polydextrose, the stability of the emulsion formed by mixing the wall material and the core material is improved through the synergistic action of the components in the wall material and the synergistic action between the wall material and the core material, the embedding rate of the prepared diglyceride microcapsule is greatly improved, and the peroxide value of the prepared microcapsule is reduced. Can effectively improve the bioavailability of the diglyceride oil and greatly broadens the application field of the diglyceride oil.
In a first aspect of the present invention, there is provided a method for preparing diglyceride microcapsules using a maillard reaction product, the method comprising the steps of: mixing wall material formed by mixing whey protein isolate, sodium caseinate, sodium starch octenyl succinate and polydextrose with diglyceride oil, and homogenizing the obtained mixture under high pressure to obtain the diglyceride microcapsule.
According to the content of the first aspect of the present invention, in some embodiments of the present invention, the whey protein isolate, the sodium caseinate, the sodium starch octenyl succinate and the polydextrose are in a ratio of (3-6): (0.5-2): (1-3): (7-9).
In some preferred embodiments of the present invention, the pH value of the wall material is 7 to 8.
In some preferred embodiments of the invention, the adjusting agent used to adjust the pH is sodium hydroxide solution.
In some preferred embodiments of the present invention, the high-pressure homogenizing pressure is 40 to 50 MPa.
In some preferred embodiments of the present invention, the number of times of the high-pressure homogenization is 2 to 3 times.
In some preferred embodiments of the present invention, the temperature of the high-pressure homogenization is 50 to 60 ℃.
In some preferred embodiments of the present invention, drying is also required after the high pressure homogenization.
In some preferred embodiments of the invention, the drying comprises spray drying.
In some more preferred embodiments of the present invention, the inlet air temperature for the spray drying is 140-200 ℃.
In some preferred embodiments of the present invention, the whey protein isolate, sodium caseinate, sodium starch octenyl succinate and polydextrose are mixed in water to form a wall material, and the water is used as a solvent.
In some preferred embodiments of the present invention, the wall material is mixed with the diglyceride oil and then subjected to a dispersion treatment.
In some more preferred embodiments of the present invention, the rotation speed of the dispersion is 8000 to 12000 r/min.
In some more preferred embodiments of the present invention, the dispersing time is 1 to 5 min.
In some preferred embodiments of the present invention, the wall material and the diglyceride oil have a mass part ratio of (1-2): 1.
according to a second aspect of the present invention, there is provided a diglyceride microcapsule prepared by the preparation method according to the first aspect of the present invention, wherein the wall material of the microcapsule is made of whey protein isolate, sodium caseinate, sodium starch octenyl succinate and polydextrose, and the core material of the microcapsule is diglyceride oil.
According to a second aspect of the present invention, in some embodiments of the invention, the diglyceride oil comprises an olive oil-derived diglyceride oil having a mass percentage of diglycerides greater than 80%.
In some preferred embodiments of the invention, the wall material is prepared from whey protein isolate, sodium caseinate, sodium starch octenyl succinate and polydextrose in parts by weight (3-6): (0.5-2): (1-3): (7-9).
In some preferred embodiments of the invention, the ratio of parts by weight of the wall material to the core material is (1-2): 1.
in a third aspect of the invention there is provided the use of a diglyceride microcapsule according to the first aspect of the invention in the preparation of a pharmaceutical formulation.
According to an aspect of the third aspect of the present invention, in some embodiments of the present invention, the drug is at least one of the following (1) to (4):
(1) a weight-reducing drug;
(2) drugs for improving blood lipid;
(3) drugs for ameliorating or treating diabetes:
(4) a medicament for treating or preventing renal disease.
The invention has the beneficial effects that:
(1) the core material is the diglyceride oil, the wall material is prepared from whey protein isolate, sodium caseinate, sodium starch octenyl succinate and polydextrose, the stability of the emulsion formed by mixing the wall material and the core material is improved through the synergistic action of the components between the wall materials and the synergistic action between the wall material and the core material, the embedding rate and the storage stability of the prepared microcapsule are greatly improved, and the peroxide value of the prepared microcapsule is reduced;
(2) the microencapsulated diglyceride oil has better water solubility, can effectively improve the bioavailability of the diglyceride oil, and greatly broadens the application field of the diglyceride oil.
Detailed Description
The invention is further described below in conjunction with specific embodiments, and the advantages and features of the invention will become more apparent as the description proceeds. These examples are illustrative only and do not limit the scope of the present invention in any way. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention, and that such changes and modifications may be made without departing from the spirit and scope of the invention.
Test materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
The specific techniques or conditions not specified in the examples can be performed according to the techniques or conditions described in the literature in the field or according to the product specification.
In an embodiment of the invention, the diglyceride oil is olive oil derived diglyceride oil having a mass percentage of diglycerides of more than 80%.
Example 1
The preparation steps of the diglyceride microcapsules are as follows:
(1) according to the mass percentage, 4.46% of whey protein isolate and 1.12% of sodium caseinate are respectively added into distilled water, the mixture is stirred for 2-3 hours, after the whey protein isolate and the sodium caseinate are completely hydrated, 2% of sodium starch octenyl succinate and 8.08% of polydextrose are sequentially added, and the mixture is rapidly and uniformly stirred at the temperature of 50-60 ℃ so that the feed liquid is fully dissolved; adjusting the pH value of the solution to 7.5 by using a sodium hydroxide solution, stirring and reacting at the temperature of 100 ℃ for 30min to fully perform the Maillard reaction, wherein the obtained Maillard reaction product is the wall material, and standing for later use;
(2) adding the diglyceride oil into the wall material, and uniformly stirring, wherein the mass ratio of the diglyceride oil to the wall material is 1: 1;
(3) dispersing the mixture of the diglyceride oil and the wall material obtained in the step (2) at a high speed for 3min under the condition of the rotating speed of 10000r/min to obtain an emulsion;
(4) homogenizing the emulsion obtained in the step (3) twice through a high-pressure homogenizer at 50-60 ℃ and 45 MPa;
(5) and (4) carrying out spray drying on the emulsion obtained in the step (4), wherein the air inlet temperature is 160 ℃, and finally obtaining the powdery diglyceride microcapsule.
Example 2
The preparation steps of the diglyceride microcapsules are as follows:
(1) according to the mass percentage, 4.46% of whey protein isolate and 1.12% of sodium caseinate are respectively added into distilled water, the mixture is stirred for 2-3 hours, after the whey protein isolate and the sodium caseinate are completely hydrated, 2% of sodium starch octenyl succinate and 8.08% of polydextrose are sequentially added, and the mixture is rapidly and uniformly stirred at the temperature of 50-60 ℃ so that the feed liquid is fully dissolved; adjusting the pH value of the solution to 7.5 by using a sodium hydroxide solution, stirring and reacting at the temperature of 100 ℃ for 30min to fully perform the Maillard reaction, wherein the obtained Maillard reaction product is the wall material, and standing for later use;
(2) adding the diglyceride oil into the wall material, and uniformly stirring, wherein the mass ratio of the diglyceride oil to the wall material is 1: 1;
(3) dispersing the mixture of the diglyceride oil and the wall material obtained in the step (2) at a high speed for 3min under the condition of the rotating speed of 10000r/min to obtain an emulsion;
(4) homogenizing the emulsion obtained in the step (3) twice through a high-pressure homogenizer at 50-60 ℃ and 45 MPa;
(5) and (4) carrying out spray drying on the emulsion obtained in the step (4), wherein the air inlet temperature is 140 ℃, and finally obtaining the powdery diglyceride microcapsule.
Example 3
The preparation steps of the diglyceride microcapsules are as follows:
(1) according to the mass percentage, 4.46% of whey protein isolate and 1.12% of sodium caseinate are respectively added into distilled water, the mixture is stirred for 2-3 hours, after the whey protein isolate and the sodium caseinate are completely hydrated, 2% of sodium starch octenyl succinate and 8.08% of polydextrose are sequentially added, and the mixture is rapidly and uniformly stirred at the temperature of 50-60 ℃ so that the feed liquid is fully dissolved; adjusting the pH value of the solution to 7.5 by using a sodium hydroxide solution, stirring and reacting at the temperature of 100 ℃ for 30min to fully perform the Maillard reaction, wherein the obtained Maillard reaction product is the wall material, and standing for later use;
(2) adding the diglyceride oil into the wall material, and fully and uniformly stirring, wherein the mass ratio of the diglyceride oil to the wall material is 1: 1;
(3) dispersing the mixture of the diglyceride oil and the wall material obtained in the step (2) at a high speed for 3min under the condition of the rotating speed of 10000r/min to obtain an emulsion;
(4) homogenizing the emulsion obtained in the step (3) twice through a high-pressure homogenizer at 50-60 ℃ and 45 MPa;
(5) and (4) carrying out spray drying on the emulsion obtained in the step (4), wherein the air inlet temperature is 180 ℃, and finally obtaining the powdery diglyceride microcapsule.
Comparative example 1
In comparison to example 1, no sodium caseinate was added in comparative example 1.
The preparation steps of the diglyceride microcapsules are as follows:
(1) respectively adding 5.58% of whey protein isolate into distilled water according to the mass percentage, stirring for 2-3 hours, after the whey protein isolate and sodium caseinate are completely hydrated, sequentially adding 2% of sodium starch octenyl succinate and 8.08% of polydextrose, and quickly and uniformly stirring at 50-60 ℃ to fully dissolve the feed liquid; adjusting the pH value of the solution to 7.5 by using a sodium hydroxide solution, stirring and reacting at the temperature of 100 ℃ for 30min to fully perform the Maillard reaction, wherein the obtained Maillard reaction product is the wall material, and standing for later use;
(2) adding the diglyceride oil into the wall material, and uniformly stirring, wherein the mass ratio of the diglyceride oil to the wall material is 1: 1;
(3) dispersing the mixture of the diglyceride oil and the wall material obtained in the step (2) at a high speed for 3min under the condition of the rotating speed of 10000r/min to obtain an emulsion;
(4) homogenizing the emulsion obtained in the step (3) twice through a high-pressure homogenizer at 50-60 ℃ and 45 MPa;
(5) and (4) carrying out spray drying on the emulsion obtained in the step (4), wherein the air inlet temperature is 160 ℃, and finally obtaining the powdery diglyceride microcapsule.
Comparative example 2
In contrast to example 1, no sodium starch octenyl succinate was added in comparative example 2.
The preparation steps of the diglyceride microcapsules are as follows:
(1) according to the mass percentage, 4.46% of whey protein isolate and 1.12% of sodium caseinate are respectively added into distilled water, the mixture is stirred for 2-3 hours, 10.08% of polydextrose is sequentially added after the whey protein isolate and the sodium caseinate are completely hydrated, and the mixture is rapidly and uniformly stirred at 50-60 ℃ so that the feed liquid is fully dissolved; adjusting the pH value of the solution to 7.5 by using a sodium hydroxide solution, stirring and reacting at the temperature of 100 ℃ for 30min to fully perform the Maillard reaction, wherein the obtained Maillard reaction product is the wall material, and standing for later use;
(2) adding the diglyceride oil into the wall material, and uniformly stirring, wherein the mass ratio of the diglyceride oil to the wall material is 1: 1;
(3) dispersing the mixture of the diglyceride oil and the wall material obtained in the step (2) at a high speed for 3min under the condition of the rotating speed of 10000r/min to obtain an emulsion;
(4) homogenizing the emulsion obtained in the step (3) twice through a high-pressure homogenizer at 50-60 ℃ and 45 MPa;
(5) and (4) carrying out spray drying on the emulsion obtained in the step (4), wherein the air inlet temperature is 160 ℃, and finally obtaining the powdery diglyceride microcapsule.
Comparative example 3
Comparative example 3 differs from example 1 in that polydextrose is replaced by an equal amount of glucose.
The preparation steps of the diglyceride microcapsules are as follows:
(1) according to the mass percentage, 4.46% of whey protein isolate and 1.12% of sodium caseinate are respectively added into distilled water, the mixture is stirred for 2-3 hours, after the whey protein isolate and the sodium caseinate are completely hydrated, 2% of sodium starch octenyl succinate and 8.08% of glucose are sequentially added, and the mixture is rapidly and uniformly stirred at the temperature of 50-60 ℃ so that the feed liquid is fully dissolved; adjusting the pH value of the solution to 7.5 by using a sodium hydroxide solution, stirring and reacting at the temperature of 100 ℃ for 30min to fully perform the Maillard reaction, wherein the obtained Maillard reaction product is the wall material, and standing for later use;
(2) adding the diglyceride oil into the wall material, and uniformly stirring, wherein the mass ratio of the diglyceride oil to the wall material is 1: 1;
(3) dispersing the mixture of the diglyceride oil and the wall material obtained in the step (2) at a high speed for 3min under the condition of the rotating speed of 10000r/min to obtain an emulsion;
(4) homogenizing the emulsion obtained in the step (3) twice through a high-pressure homogenizer at 50-60 ℃ and 45 MPa;
(5) and (5) carrying out spray drying on the emulsion obtained in the step (4) at the air inlet temperature of 160 ℃, and finally preparing the powdery diglyceride microcapsule.
Comparative example 4
Comparative example 4 is different from example 1 in that polydextrose is replaced by an equal amount of maltodextrin.
The preparation steps of the diglyceride microcapsules are as follows:
(1) according to the mass percentage, 4.46% of whey protein isolate and 1.12% of sodium caseinate are respectively added into distilled water, the mixture is stirred for 2-3 hours, after the whey protein isolate and the sodium caseinate are completely hydrated, 2% of sodium starch octenyl succinate and 8.08% of maltodextrin are sequentially added, and the mixture is rapidly and uniformly stirred at 50-60 ℃ so that the feed liquid is fully dissolved; adjusting the pH value of the solution to 7.5 by using a sodium hydroxide solution, stirring and reacting at the temperature of 100 ℃ for 30min to fully perform the Maillard reaction, wherein the obtained Maillard reaction product is the wall material, and standing for later use;
(2) and adding the diglyceride oil into the wall materials, and uniformly stirring, wherein the mass ratio of the diglyceride oil to the wall materials is 1: 1;
(3) dispersing the mixture of the diglyceride oil and the wall material obtained in the step (2) at a high speed for 3min under the condition of the rotating speed of 10000r/min to obtain an emulsion;
(4) homogenizing the emulsion obtained in the step (3) twice through a high-pressure homogenizer at 50-60 ℃ and 45 MPa;
(5) and (4) carrying out spray drying on the emulsion obtained in the step (4), wherein the air inlet temperature is 160 ℃, and finally obtaining the powdery diglyceride microcapsule.
Comparative example 5
The difference between comparative example 5 and example 1 is that the ratio of whey protein isolate and sodium caseinate was adjusted.
The preparation steps of the diglyceride microcapsules are as follows:
(1) according to the mass percentage, 2.79% of whey protein isolate and 2.79% of sodium caseinate are respectively added into distilled water, the mixture is stirred for 2-3 hours, after the whey protein isolate and the sodium caseinate are completely hydrated, 2% of sodium starch octenyl succinate and 8.08% of polydextrose are sequentially added, and the mixture is rapidly and uniformly stirred at the temperature of 50-60 ℃ so that the feed liquid is fully dissolved; adjusting the pH value of the solution to 7.5 by using a sodium hydroxide solution, stirring and reacting at the temperature of 100 ℃ for 30min to fully perform the Maillard reaction, wherein the obtained Maillard reaction product is the wall material, and standing for later use;
(2) adding the diglyceride oil into the wall material, and uniformly stirring, wherein the mass ratio of the diglyceride oil to the wall material is 1: 1;
(3) dispersing the mixture of the diglyceride oil and the wall material obtained in the step (2) at a high speed for 3min under the condition of the rotating speed of 10000r/min to obtain an emulsion;
(4) homogenizing the emulsion obtained in the step (3) twice through a high-pressure homogenizer at 50-60 ℃ and 45 MPa;
(5) and (5) carrying out spray drying on the emulsion obtained in the step (4) at the air inlet temperature of 160 ℃, and finally preparing the powdery diglyceride microcapsule.
Comparative example 6
Comparative example 6 is different from example 1 in that no pH adjustment is performed.
The preparation steps of the diglyceride microcapsules are as follows:
(1) according to the mass percentage, 4.46% of whey protein isolate and 1.12% of sodium caseinate are respectively added into distilled water, the materials are stirred for 2-3 hours, after the whey protein isolate and the sodium caseinate are completely hydrated, 2% of sodium starch octenyl succinate and 8.08% of polydextrose are sequentially added, the materials are quickly and uniformly stirred at 50-60 ℃ to fully dissolve the materials, the pH value of the materials is 6.5, the materials are stirred and react for 30min at the temperature of 100 ℃ to fully perform the Maillard reaction, the obtained Maillard reaction product is the wall material, and the wall material is placed for standby;
(2) adding the diglyceride oil into the wall material, and uniformly stirring, wherein the mass ratio of the diglyceride oil to the wall material is 1: 1;
(3) dispersing the mixture of the diglyceride oil and the wall material obtained in the step (2) at a high speed for 3min under the condition of the rotating speed of 10000r/min to obtain an emulsion;
(4) homogenizing the emulsion obtained in the step (3) twice through a high-pressure homogenizer at 50-60 ℃ and 45 MPa;
(5) and (4) carrying out spray drying on the emulsion obtained in the step (4), wherein the air inlet temperature is 160 ℃, and finally obtaining the powdery diglyceride microcapsule.
Comparative example 7
Comparative example 7 differs from example 1 in that the core material was replaced with an equal amount of pumpkin seed oil.
The preparation steps of the pumpkin seed oil microcapsule are as follows:
(1) according to the mass percentage, 4.46% of whey protein isolate and 1.12% of sodium caseinate are respectively added into distilled water, the mixture is stirred for 2-3 hours, after the whey protein isolate and the sodium caseinate are completely hydrated, 2% of sodium starch octenyl succinate and 8.08% of polydextrose are sequentially added, and the mixture is rapidly and uniformly stirred at the temperature of 50-60 ℃ so that the feed liquid is fully dissolved; adjusting the pH value of the solution to 7.5 by using a sodium hydroxide solution, stirring and reacting at the temperature of 100 ℃ for 30min to fully perform the Maillard reaction, wherein the obtained Maillard reaction product is the wall material, and standing for later use;
(2) adding pumpkin seed oil into the wall material, and uniformly stirring, wherein the mass ratio of the pumpkin seed oil to the wall material is 1: 1;
(3) dispersing the mixture of the pumpkin seed oil and the wall material obtained in the step (2) at a high speed for 3min under the condition of the rotating speed of 10000r/min to obtain emulsion;
(4) homogenizing the emulsion obtained in the step (3) twice through a high-pressure homogenizer at 50-60 ℃ and 45 MPa;
(5) and (4) carrying out spray drying on the emulsion obtained in the step (4), wherein the air inlet temperature is 160 ℃, and finally obtaining the powdery pumpkin seed oil microcapsule.
Example of detection
The specific method of the test involved in the embodiment of the invention comprises the following steps:
(1) stability testing of the emulsions: the stability of the emulsion is characterized by The Stability Index (TSI) of the emulsion system, and the dynamic changes of the emulsion system are monitored by the intensity of the backscattered light and the transmitted light by using a stability analyzer to vertically scan the emulsion sample before spray drying in a top-down manner. 20mL of the emulsion sample was added to a glass vial dedicated to a Turbiscan Lab Expert multiple light scattering instrument, the temperature was set at 30 ℃ and the scan was performed 1 time every 2min for 2h, and the sample scan was recorded and the measurement was repeated 3 times. The data was analyzed using Turbi Soft based on the change in sample transmitted light and back scattered intensity to give the TSI of the emulsion.
(2) And (3) testing the embedding rate: the quality of the microcapsule surface oil was measured according to the method specified in QBT 4791-2015. The total oil quality of the microcapsules was determined according to the method specified in GB 5009.6-2016. The embedding rate of the microcapsules is calculated by the following formula:
Figure BDA0003619000340000081
(3) solubility test: accurately weighing 1g of microcapsules, dissolving the microcapsules in 5mL of distilled water, dissolving the samples in several times without stirring, placing the dissolved samples into a centrifuge tube for centrifugation, centrifuging for 10min at 3000r/min, taking out the supernatant, adding a proper amount of distilled water into the centrifuge tube, centrifuging again under the same condition, taking out the supernatant, repeating for several times until the mass of the precipitate in the centrifuge tube does not change, taking out the precipitate, placing the precipitate into an evaporation dish with constant weight, placing the evaporation dish in an oven at 105 ℃ for drying to constant weight, and recording the mass of the precipitateIs m Precipitation of
Solubility (g) ═ 1-m of microcapsules Precipitation of )×20×100%。
(4) Determination of peroxide number: the microcapsules were stored in an oven at 60 ℃ for 18 days and then measured according to the method specified in GB 5009.227-2016.
TABLE 1 results of tests on stability, embedding rate of microcapsules, powder color of microcapsules, solubility of microcapsules, and peroxide value of microcapsules prepared in examples 1 to 3 and comparative examples 1 to 7
Figure BDA0003619000340000091
As can be seen from Table 1, the emulsions prepared by the preparation method in the embodiment of the invention have smaller TSI values, and the TSI values are not more than 3, while the TSI values of the emulsions in comparative examples 1 to 7 are obviously higher than those of examples 1 to 3. The smaller the value of TSI is, the higher the stability of the emulsion is, that is, compared to the comparative example, the stability of the emulsion composed of the wall material and the core material in the embodiment of the present invention is better, which indicates that the emulsification effect of the wall material in the embodiment of the present invention is better, so that the embedding rate of the prepared microcapsule is improved, the microcapsule in the embodiment of the present invention has a higher embedding rate, the embedding rate is all over 97%, while the embedding rate of the microcapsules in comparative examples 1 to 7 is lower, and the embedding rate of the microcapsule in comparative example 5 is only 90.06%. In addition, as can be seen from Table 1, the peroxide values in examples 1 to 3 are all less than 6meq/kg, and in contrast, the peroxide values in comparative examples 1 to 7 are all more than 6meq/kg, which indicates that the microcapsules prepared in the examples of the present invention have strong storage stability. Compared with the example 1, the embedding rate in the comparative example 1 is lower, and the peroxide value is higher, which shows that compared with the method of using whey protein isolate alone as an emulsifier, the compound of whey protein isolate and sodium caseinate can generate a synergistic effect, so that the emulsifying capacity can be enhanced, and further, the embedding rate of the prepared microcapsule is improved, and the peroxide value of the microcapsule is reduced. As can be seen from the data of comparative example 5, adjusting the ratio of whey protein isolate to sodium caseinate has a great influence on the embedding rate of the microcapsules, indicating that the whey protein isolate and sodium caseinate can exert better synergistic effect only by compounding in an atmosphere with proper ratio. Compared with example 1, the peroxide value in comparative example 2 is greatly improved when no sodium starch octenyl succinate is added in comparative example 2, which shows that the peroxide value of the prepared microcapsule can be reduced by matching sodium starch octenyl succinate with other components. It can be seen from the data of comparative examples 3 and 4 that polydextrose has a large influence on the performance of the microcapsules prepared according to the present invention, the performance of the microcapsules prepared can be improved by the synergistic cooperation of polydextrose and other components, and the encapsulation efficiency and storage stability of the microcapsules prepared are significantly reduced after polydextrose is replaced with glucose or maltodextrin. In the comparative example 6, the pH value is not adjusted, and the embedding rate of the prepared microcapsule is reduced, which shows that the adjustment of the pH value is a key technology of the Maillard reaction of the wall material solution, and the adjustment of the pH value is beneficial to the completion of the Maillard reaction, thereby improving the embedding rate of the microcapsule. In comparative example 7, the oil embedded in the microcapsule is changed, and the core material is changed from diglyceride oil to pumpkin seed oil, so that the embedding rate and the storage stability of the prepared microcapsule are reduced, and the core material and the wall material in the embodiment of the invention have better synergistic effect.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.

Claims (10)

1. A method for preparing diglyceride microcapsules using maillard reaction products, comprising the steps of: mixing wall material formed by mixing whey protein isolate, sodium caseinate, sodium starch octenyl succinate and polydextrose with diglyceride oil, and homogenizing the obtained mixture under high pressure to obtain diglyceride microcapsules; wherein the whey protein isolate, the sodium caseinate, the sodium starch octenyl succinate and the polydextrose are in a mass part ratio of (3-6): (0.5-2): (1-3): (7-9), wherein the pH value of the wall material is 7-8.
2. The method according to claim 1, wherein the pressure of the high-pressure homogenization is 40-50 MPa, and the number of times of the high-pressure homogenization is 2-3 times.
3. The method according to claim 1, wherein the temperature of the high-pressure homogenization is 50-60 ℃.
4. The method according to claim 1, wherein drying is further required after the high-pressure homogenization, wherein the drying method is spray drying, and the inlet air temperature of the spray drying is 140-200 ℃.
5. The method of claim 1 wherein the wall material is mixed with the diglyceride oil prior to the dispersing step.
6. The method according to claim 5, wherein the rotation speed of the dispersion is 8000-12000 r/min, and the dispersion time is 1-5 min.
7. The method according to claim 1, wherein the mass part ratio of the wall material to the diglyceride oil in the diglyceride microcapsules is (1-2): 1.
8. diglyceride microcapsules prepared according to any of claims 1 to 7, wherein the wall material of the microcapsules is prepared from whey protein isolate, sodium caseinate, sodium starch octenyl succinate and polydextrose, and the core material of the microcapsules is diglyceride oil.
9. The microcapsule according to claim 8, wherein the wall material is prepared from whey protein isolate, sodium caseinate, sodium starch octenyl succinate and polydextrose in a mass ratio of (3-6): (0.5-2): (1-3): (7-9), wherein the wall material and the core material are in a mass part ratio of (1-2): 1.
10. use of the diglyceride microcapsules of any one of claims 1 to 7 for producing a pharmaceutical preparation, wherein the drug is at least one of the following (1) to (4):
(1) a weight-reducing drug;
(2) drugs for improving blood lipid;
(3) drugs for ameliorating or treating diabetes:
(4) a medicament for treating or preventing renal disease.
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