CN114831957B - Diglyceride microcapsule prepared by Maillard reaction product and preparation method thereof - Google Patents

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

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CN114831957B
CN114831957B CN202210451974.6A CN202210451974A CN114831957B CN 114831957 B CN114831957 B CN 114831957B CN 202210451974 A CN202210451974 A CN 202210451974A CN 114831957 B CN114831957 B CN 114831957B
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diglyceride
microcapsule
wall material
whey protein
protein isolate
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CN114831957A (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
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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    • 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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  • Manufacturing Of Micro-Capsules (AREA)

Abstract

The invention discloses a diglyceride microcapsule prepared by Maillard reaction products and a preparation method thereof. The method comprises the following steps: mixing wall materials 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 mass part ratio of whey protein isolate, sodium caseinate, sodium starch octenyl succinate and polydextrose is (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, through the synergistic effect of all components in the wall material and the synergistic effect between the wall material and the core material, the stability of emulsion formed after the wall material and the core material are mixed is improved, and the embedding rate and the storage stability of the prepared diglyceride microcapsule are greatly improved.

Description

Diglyceride microcapsule prepared by 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
The diglyceride oil is a functional grease, and is a product obtained by esterification reaction of two hydroxyl groups in glycerol and fatty acid. In recent years, researches 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 mellitus and kidney disease, and the like, and thus has been receiving attention. The unique metabolic characteristics of diglyceride oils are believed to be responsible for their specific physiological functions. The decomposition products of diglyceride in 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 by 2-monoglyceride to obtain triglyceride, thereby reducing the accumulation of triglyceride. In addition, ingestion of diglyceride oil promotes the activity of enzymes associated with beta oxidation, which promotes the decomposition of free fatty acids, thereby reducing the re-synthesis of triglycerides in the body, reducing triglycerides in the blood circulation, and reducing blood lipid levels and fat accumulation.
However, liquid diglyceride oils have the disadvantages of poor stability, poor solubility in water, low oral availability, etc., limiting the usability of the diglyceride oil in food products. To overcome these drawbacks, encapsulation of functional oils into emulsion-based microcapsule systems is a potential approach. The microcapsule can pulverize liquid diglyceride oil, can keep original characteristics, performances and biological activities of the diglyceride oil to the greatest extent through morphological change and active substance release regulation, can effectively prevent oxidation of the diglyceride oil and volatilization of flavor substances, and effectively avoid reaction of the diglyceride oil and the external environment, thereby effectively preventing damage and loss of nutrient substances in the diglyceride oil. Therefore, finding a wall material suitable for diglyceride oil has important research significance, and is beneficial to widening the application field of the diglyceride oil.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems in the prior art described above. Therefore, the invention provides a diglyceride microcapsule prepared by utilizing 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, and the stability of emulsion formed by mixing the wall material and the core material is improved through the synergistic effect of all components in the wall material and the synergistic effect between the wall material and the core material, so that 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 widen the application field of the diglyceride oil.
In a first aspect of the present invention, there is provided a process for preparing diglyceride microcapsules using a maillard reaction product, the process comprising the steps of: mixing wall materials 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 first aspect of the present invention, in some embodiments of the present invention, the whey protein isolate, sodium caseinate, sodium starch octenyl succinate and polydextrose are in the mass ratio of (3-6): (0.5-2): (1-3): (7-9).
In some preferred embodiments of the invention, the pH of the wall material is 7 to 8.
In some preferred embodiments of the invention, the regulator used to adjust the pH is sodium hydroxide solution.
In some preferred embodiments of the invention, the high pressure homogenization is at a pressure of 40 to 50MPa.
In some preferred embodiments of the invention, the number of high pressure homogenizations is 2 to 3.
In some preferred embodiments of the invention, the high pressure homogenisation temperature is in the range 50 to 60 ℃.
In some preferred embodiments of the 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 invention, the spray-dried inlet air temperature is 140-200 ℃.
In some preferred embodiments of the 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 invention, the wall material is further subjected to a dispersion treatment after mixing with the diglyceride oil.
In some more preferred embodiments of the invention, the rotational speed of the dispersion is 8000 to 12000r/min.
In some more preferred embodiments of the invention, the time of dispersion is from 1 to 5 minutes.
In some preferred embodiments of the present invention, the mass part ratio of the wall material to the diglyceride oil is (1-2): 1.
according to the second aspect of the invention, the diglyceride microcapsule prepared by the preparation method of the first aspect is provided, the wall material of the microcapsule is prepared from 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 invention, in some embodiments of the invention, the diglyceride oil comprises a source of olive oil having a mass percentage of diglycerides of greater than 80%.
In some preferred embodiments of the present invention, the weight part ratio of whey protein isolate, sodium caseinate, sodium starch octenyl succinate and polydextrose in the preparation raw materials of the wall material is (3-6): (0.5-2): (1-3): (7-9).
In some preferred embodiments of the present invention, the mass part ratio 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 manufacture of a pharmaceutical formulation.
According to a 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) A medicament for improving blood fat;
(3) Drugs for improving or treating diabetes:
(4) A medicament for treating or preventing kidney disease.
The invention has the beneficial effects that:
(1) The core material is diglyceride oil, the wall material is prepared from whey protein isolate, sodium caseinate, sodium starch octenyl succinate and polydextrose, and the stability of emulsion formed by mixing the wall material and the core material is improved by the synergistic effect of all components among the wall materials and the synergistic effect between the wall material and the core material, so that the embedding rate and 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 widens the application field of the diglyceride oil.
Detailed Description
The invention will be further described with reference to specific embodiments, and advantages and features of the invention will become apparent from the description. These examples are merely exemplary and do not limit the scope of the invention in any way. It will be understood by those skilled in the art that various changes and substitutions of details and forms of the technical solution of the present invention may be made without departing from the spirit and scope of the present invention, but these changes and substitutions fall within the scope of the present invention.
The test materials, reagents and the like used in the examples described below are commercially available unless otherwise specified.
Those of skill in the art, without any particular mention of the techniques or conditions, may follow the techniques or conditions described in the literature in this field or follow the product specifications.
In an embodiment of the present invention, the diglyceride oil is an olive oil-derived diglyceride oil having a mass percentage of diglycerides of more than 80%.
Example 1
The preparation steps of the diglyceride microcapsule are as follows:
(1) According to the mass percent, 4.46 percent of whey protein isolate and 1.12 percent of sodium caseinate are respectively added into distilled water, and stirred for 2 to 3 hours, after the whey protein isolate and the sodium caseinate are completely water-mixed, 2 percent of sodium starch octenyl succinate and 8.08 percent of polydextrose are sequentially added, and the materials are rapidly and uniformly stirred at 50 to 60 ℃ to ensure that the materials are fully dissolved; adjusting the pH of the solution to 7.5 by using sodium hydroxide solution, stirring and reacting for 30min at the temperature of 100 ℃ to fully perform Maillard reaction, wherein the obtained Maillard reaction product is a wall material, and standing for later use;
(2) Adding diglyceride oil into the wall material, and uniformly stirring, wherein the mass ratio of the diglyceride oil to the wall material is 1:1, a step of;
(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 rotating speed condition of 10000r/min to obtain emulsion;
(4) Homogenizing the emulsion obtained in the step (3) twice by a high-pressure homogenizer at 50-60 ℃ and 45 MPa;
(5) And (3) spray drying the emulsion obtained in the step (4), wherein the air inlet temperature is 160 ℃, and finally, the powdery diglyceride microcapsule is prepared.
Example 2
The preparation steps of the diglyceride microcapsule are as follows:
(1) According to the mass percent, 4.46 percent of whey protein isolate and 1.12 percent of sodium caseinate are respectively added into distilled water, and stirred for 2 to 3 hours, after the whey protein isolate and the sodium caseinate are completely water-mixed, 2 percent of sodium starch octenyl succinate and 8.08 percent of polydextrose are sequentially added, and the materials are rapidly and uniformly stirred at 50 to 60 ℃ to ensure that the materials are fully dissolved; adjusting the pH of the solution to 7.5 by using sodium hydroxide solution, stirring and reacting for 30min at the temperature of 100 ℃ to fully perform Maillard reaction, wherein the obtained Maillard reaction product is a wall material, and standing for later use;
(2) Adding diglyceride oil into the wall material, and uniformly stirring, wherein the mass ratio of the diglyceride oil to the wall material is 1:1, a step of;
(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 rotating speed condition of 10000r/min to obtain emulsion;
(4) Homogenizing the emulsion obtained in the step (3) twice by a high-pressure homogenizer at 50-60 ℃ and 45 MPa;
(5) And (3) spray drying the emulsion obtained in the step (4), wherein the air inlet temperature is 140 ℃, and finally, the powdery diglyceride microcapsule is prepared.
Example 3
The preparation steps of the diglyceride microcapsule are as follows:
(1) According to the mass percent, 4.46 percent of whey protein isolate and 1.12 percent of sodium caseinate are respectively added into distilled water, and stirred for 2 to 3 hours, after the whey protein isolate and the sodium caseinate are completely water-mixed, 2 percent of sodium starch octenyl succinate and 8.08 percent of polydextrose are sequentially added, and the materials are rapidly and uniformly stirred at 50 to 60 ℃ to ensure that the materials are fully dissolved; adjusting the pH of the solution to 7.5 by using sodium hydroxide solution, stirring and reacting for 30min at the temperature of 100 ℃ to fully perform Maillard reaction, wherein the obtained Maillard reaction product is a wall material, and standing for later use;
(2) Adding 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, a step of;
(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 rotating speed condition of 10000r/min to obtain emulsion;
(4) Homogenizing the emulsion obtained in the step (3) twice by a high-pressure homogenizer at 50-60 ℃ and 45 MPa;
(5) And (3) spray drying the emulsion obtained in the step (4), wherein the air inlet temperature is 180 ℃, and finally, the powdery diglyceride microcapsule is prepared.
Comparative example 1
In comparison with example 1, sodium caseinate was not added in comparative example 1.
The preparation steps of the diglyceride microcapsule are as follows:
(1) According to the mass percentage, respectively adding 5.58% of whey protein isolate into distilled water, stirring for 2-3 hours, after the whey protein isolate and sodium caseinate are completely water-added, sequentially adding 2% of sodium starch octenyl succinate and 8.08% of polydextrose, and rapidly and uniformly stirring at 50-60 ℃ to enable the feed liquid to be fully dissolved; adjusting the pH of the solution to 7.5 by using sodium hydroxide solution, stirring and reacting for 30min at the temperature of 100 ℃ to fully perform Maillard reaction, wherein the obtained Maillard reaction product is a wall material, and standing for later use;
(2) Adding diglyceride oil into the wall material, and uniformly stirring, wherein the mass ratio of the diglyceride oil to the wall material is 1:1, a step of;
(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 rotating speed condition of 10000r/min to obtain emulsion;
(4) Homogenizing the emulsion obtained in the step (3) twice by a high-pressure homogenizer at 50-60 ℃ and 45 MPa;
(5) And (3) spray drying the emulsion obtained in the step (4), wherein the air inlet temperature is 160 ℃, and finally, the powdery diglyceride microcapsule is prepared.
Comparative example 2
In comparison with example 1, sodium starch octenyl succinate was not added to comparative example 2.
The preparation steps of the diglyceride microcapsule are as follows:
(1) According to the mass percent, 4.46 percent of whey protein isolate and 1.12 percent of sodium caseinate are respectively added into distilled water, and stirred for 2 to 3 hours, after the whey protein isolate and the sodium caseinate are completely water-mixed, 10.08 percent of polydextrose is sequentially added, and the materials are rapidly and uniformly stirred at 50 to 60 ℃ to ensure that the feed liquid is fully dissolved; adjusting the pH of the solution to 7.5 by using sodium hydroxide solution, stirring and reacting for 30min at the temperature of 100 ℃ to fully perform Maillard reaction, wherein the obtained Maillard reaction product is a wall material, and standing for later use;
(2) Adding diglyceride oil into the wall material, and uniformly stirring, wherein the mass ratio of the diglyceride oil to the wall material is 1:1, a step of;
(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 rotating speed condition of 10000r/min to obtain emulsion;
(4) Homogenizing the emulsion obtained in the step (3) twice by a high-pressure homogenizer at 50-60 ℃ and 45 MPa;
(5) And (3) spray drying the emulsion obtained in the step (4), wherein the air inlet temperature is 160 ℃, and finally, the powdery diglyceride microcapsule is prepared.
Comparative example 3
Comparative example 3 differs from example 1 in that polydextrose was replaced with an equal amount of glucose.
The preparation steps of the diglyceride microcapsule are as follows:
(1) According to the mass percent, 4.46 percent of whey protein isolate and 1.12 percent of sodium caseinate are respectively added into distilled water, and stirred for 2 to 3 hours, after the whey protein isolate and the sodium caseinate are completely water-mixed, 2 percent of sodium starch octenyl succinate and 8.08 percent of glucose are sequentially added, and the materials are rapidly and uniformly stirred at 50 to 60 ℃ to ensure that the materials are fully dissolved; adjusting the pH of the solution to 7.5 by using sodium hydroxide solution, stirring and reacting for 30min at the temperature of 100 ℃ to fully perform Maillard reaction, wherein the obtained Maillard reaction product is a wall material, and standing for later use;
(2) Adding diglyceride oil into the wall material, and uniformly stirring, wherein the mass ratio of the diglyceride oil to the wall material is 1:1, a step of;
(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 rotating speed condition of 10000r/min to obtain emulsion;
(4) Homogenizing the emulsion obtained in the step (3) twice by a high-pressure homogenizer at 50-60 ℃ and 45 MPa;
(5) And (3) spray drying the emulsion obtained in the step (4), wherein the air inlet temperature is 160 ℃, and finally, the powdery diglyceride microcapsule is prepared.
Comparative example 4
Comparative example 4 differs from example 1 in that polydextrose was replaced with an equivalent amount of maltodextrin.
The preparation steps of the diglyceride microcapsule are as follows:
(1) According to the mass percent, 4.46 percent of whey protein isolate and 1.12 percent of sodium caseinate are respectively added into distilled water, and stirred for 2 to 3 hours, after the whey protein isolate and the sodium caseinate are completely water-mixed, 2 percent of sodium starch octenyl succinate and 8.08 percent of maltodextrin are sequentially added, and the materials are rapidly and uniformly stirred at 50 to 60 ℃ to ensure that the materials are fully dissolved; adjusting the pH of the solution to 7.5 by using sodium hydroxide solution, stirring and reacting for 30min at the temperature of 100 ℃ to fully perform Maillard reaction, wherein the obtained Maillard reaction product is a wall material, and standing for later use;
(2) Adding diglyceride oil into the wall material, and uniformly stirring, wherein the mass ratio of the diglyceride oil to the wall material is 1:1, a step of;
(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 rotating speed condition of 10000r/min to obtain emulsion;
(4) Homogenizing the emulsion obtained in the step (3) twice by a high-pressure homogenizer at 50-60 ℃ and 45 MPa;
(5) And (3) spray drying the emulsion obtained in the step (4), wherein the air inlet temperature is 160 ℃, and finally, the powdery diglyceride microcapsule is prepared.
Comparative example 5
Comparative example 5 differs from example 1 in that the ratio of whey protein isolate to sodium caseinate was adjusted.
The preparation steps of the diglyceride microcapsule are as follows:
(1) According to the mass percent, 2.79 percent of whey protein isolate and 2.79 percent of sodium caseinate are respectively added into distilled water, and stirred for 2 to 3 hours, after the whey protein isolate and the sodium caseinate are completely water-mixed, 2 percent of sodium starch octenyl succinate and 8.08 percent of polydextrose are sequentially added, and the materials are rapidly and uniformly stirred at 50 to 60 ℃ to ensure that the materials are fully dissolved; adjusting the pH of the solution to 7.5 by using sodium hydroxide solution, stirring and reacting for 30min at the temperature of 100 ℃ to fully perform Maillard reaction, wherein the obtained Maillard reaction product is a wall material, and standing for later use;
(2) Adding diglyceride oil into the wall material, and uniformly stirring, wherein the mass ratio of the diglyceride oil to the wall material is 1:1, a step of;
(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 rotating speed condition of 10000r/min to obtain emulsion;
(4) Homogenizing the emulsion obtained in the step (3) twice by a high-pressure homogenizer at 50-60 ℃ and 45 MPa;
(5) And (3) spray drying the emulsion obtained in the step (4), wherein the air inlet temperature is 160 ℃, and finally, the powdery diglyceride microcapsule is prepared.
Comparative example 6
Comparative example 6 differs from example 1 in that no pH adjustment was performed.
The preparation steps of the diglyceride microcapsule are as follows:
(1) According to the mass percent, 4.46 percent of whey protein isolate and 1.12 percent of sodium caseinate are respectively added into distilled water, stirred for 2 to 3 hours, after the whey protein isolate and the sodium caseinate are completely water-mixed, 2 percent of sodium starch octenyl succinate and 8.08 percent of polydextrose are sequentially added, and the materials are rapidly and uniformly stirred at 50 to 60 ℃ to ensure that the material liquid is fully dissolved, the pH value is 6.5, and the stirring reaction is carried out for 30 minutes at the temperature of 100 ℃ to ensure that the Maillard reaction is fully carried out, and the obtained Maillard reaction product is a wall material and is placed for standby;
(2) Adding diglyceride oil into the wall material, and uniformly stirring, wherein the mass ratio of the diglyceride oil to the wall material is 1:1, a step of;
(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 rotating speed condition of 10000r/min to obtain emulsion;
(4) Homogenizing the emulsion obtained in the step (3) twice by a high-pressure homogenizer at 50-60 ℃ and 45 MPa;
(5) And (3) spray drying the emulsion obtained in the step (4), wherein the air inlet temperature is 160 ℃, and finally, the powdery diglyceride microcapsule is prepared.
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 method of the pumpkin seed oil microcapsule comprises the following steps:
(1) According to the mass percent, 4.46 percent of whey protein isolate and 1.12 percent of sodium caseinate are respectively added into distilled water, and stirred for 2 to 3 hours, after the whey protein isolate and the sodium caseinate are completely water-mixed, 2 percent of sodium starch octenyl succinate and 8.08 percent of polydextrose are sequentially added, and the materials are rapidly and uniformly stirred at 50 to 60 ℃ to ensure that the materials are fully dissolved; adjusting the pH of the solution to 7.5 by using sodium hydroxide solution, stirring and reacting for 30min at the temperature of 100 ℃ to fully perform Maillard reaction, wherein the obtained Maillard reaction product is a 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, a step of;
(3) Dispersing the mixture of pumpkin seed oil and wall materials obtained in the step (2) at a high speed for 3min under the rotating speed condition of 10000r/min to obtain emulsion;
(4) Homogenizing the emulsion obtained in the step (3) twice by a high-pressure homogenizer at 50-60 ℃ and 45 MPa;
(5) And (3) spray drying the emulsion obtained in the step (4) to obtain the powdery pumpkin seed oil microcapsule, wherein the air inlet temperature is 160 ℃.
Test case
The specific method for testing the embodiment of the invention comprises the following steps:
(1) Stability test of emulsion: emulsion stability is characterized by The Stability Index (TSI) of the emulsion system, which is monitored for dynamic changes by back-scattered light intensity and transmitted light using a stability analyzer to perform a top-down vertical scan of the emulsion sample prior to spray drying. 20mL of the emulsion sample is added into a special glass bottle of a Turbiscan Lab Expert multiple light scattering instrument, the temperature is set to 30 ℃, the scanning is performed for 1 time every 2min for 2h, the scanning pattern of the sample is recorded, and the measurement is repeated for 3 times. Based on the changes in transmitted light and back-scattered intensity of the samples, the data were analyzed using a turbo Soft to obtain the TSI of the emulsion.
(2) And (3) testing embedding rate: the mass of oil on the microcapsule surface was determined according to the method specified in QBT 4791-2015. The total oil mass of the microcapsules was determined according to the method specified in GB 5009.6-2016. The encapsulation efficiency of the microcapsules was calculated by the following formula:
Figure BDA0003619000340000081
(3) Solubility test: accurately weighing 1g of microcapsule, dissolving in 5mL of distilled water, stirring for dissolving several times, centrifuging the dissolved sample in a centrifuge tube for 10min at 3000r/min, taking out the supernatant, adding appropriate 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 precipitate in the centrifuge tube is unchanged, taking out the precipitate, placing the precipitate in a constant-weight evaporating dish, drying in an oven at 105 ℃ until the mass of precipitate is constant, and recording the mass of precipitate as m Precipitation
Solubility of microcapsules (g) = (1-m) Precipitation )×20×100%。
(4) Measurement of peroxide value: 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 for stability of emulsion, encapsulation efficiency of microcapsule, color of microcapsule powder, solubility of microcapsule and peroxide value of microcapsule prepared in examples 1 to 3 and comparative examples 1 to 7
Figure BDA0003619000340000091
As can be seen from Table 1, the emulsions prepared using the preparation method of the examples of the present invention had smaller TSI values, neither TSI value exceeding 3, but the TSI values of the emulsions of comparative examples 1 to 7 were significantly higher than those of examples 1 to 3. The smaller the TSI value, the higher the stability of the emulsion, that is, the better the stability of the emulsion composed of the wall material and the core material in the embodiment of the present invention compared with the comparative example, which shows that the wall material in the embodiment of the present invention has a better emulsification effect, thereby improving the embedding rate of the prepared microcapsule, the microcapsule in the embodiment of the present invention has a higher embedding rate, the embedding rate is more than 97%, 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, it can be seen from Table 1 that the peroxide values in examples 1 to 3 were each less than 6meq/kg, whereas the peroxide values in comparative examples 1 to 7 were each more than 6meq/kg, indicating that the microcapsules prepared in the examples of the present invention had a strong storage stability. The lower embedding rate and higher peroxide value of comparative example 1 compared with those of comparative example 1 indicate that the synergistic effect of whey protein isolate and sodium caseinate is generated after compounding, which can enhance the emulsifying capacity, further improve the embedding rate of the prepared microcapsule and reduce the peroxide value of the microcapsule compared with the case of using whey protein isolate alone as the emulsifier. From the data of comparative example 5, it can be seen that adjusting the ratio of whey protein isolate and sodium caseinate has a larger effect on the entrapment rate of the microcapsules, indicating that whey protein isolate and sodium caseinate can exert better synergistic effect only by compounding in a proper ratio atmosphere. The sodium starch octenyl succinate is not added in comparative example 2, but the peroxide value is greatly increased in comparative example 2, compared with example 1, indicating that the blending of sodium starch octenyl succinate with other components can act to reduce the peroxide value of the prepared microcapsules. As can be seen from the data of comparative examples 3 and 4, the polydextrose has a great influence on the performance of the microcapsules prepared by the present invention, and the performance of the prepared microcapsules can be improved by the synergistic combination of polydextrose and other components, and the entrapment rate and storage stability of the prepared microcapsules are remarkably reduced after the polydextrose is replaced by glucose or maltodextrin. In comparative example 6, the prepared microcapsule had a decreased entrapment rate without pH adjustment, indicating that pH adjustment is a key technique for maillard reaction of wall material solution, and the pH adjustment is advantageous for complete maillard reaction, thereby increasing the entrapment rate of the microcapsule. In comparative example 7, the oil embedded in the microcapsule was replaced, and the core material was replaced with pumpkin seed oil from diglyceride oil, and the embedding rate and storage stability of the prepared microcapsule were both reduced, indicating that the core material and the wall material in the examples of the present invention have good synergistic effect.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.

Claims (10)

1. A method for preparing diglyceride microcapsules by using maillard reaction products, the method comprising the steps of: mixing wall materials 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 mass part ratio of the whey protein isolate to the sodium caseinate is 4.46:1.12, wherein the pH value of the wall material is 7.5.
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 of claim 1, wherein the high pressure homogenization temperature is 50-60 ℃.
4. The method of claim 1, further comprising drying after the high pressure homogenizing, wherein the drying 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 further subjected to a dispersion treatment after mixing with the diglyceride oil.
6. The method of claim 5, wherein the dispersing speed is 8000-12000 r/min and the dispersing time is 1-5 min.
7. The method of claim 1, wherein the mass ratio of the wall material and the diglyceride oil in the diglyceride microcapsule is (1-2): 1.
8. the diglyceride microcapsule prepared by the method according to any one of claims 1 to 7, wherein the wall material of the microcapsule is prepared from whey protein isolate, sodium caseinate, sodium starch octenyl succinate and polydextrose, and the core material of the microcapsule is diglyceride oil.
9. The microcapsule according to claim 8, wherein the weight ratio of whey protein isolate to sodium caseinate in the preparation raw material of the wall material is 4.46:1.12, wherein the mass ratio of the wall material to the core material is (1-2): 1.
10. use of the diglyceride microcapsule according to any one of claims 1 to 7 in the preparation of a pharmaceutical formulation, wherein the medicament is at least one of the following (1) to (4):
(1) A weight-reducing drug;
(2) A medicament for improving blood fat;
(3) A medicament for improving or treating diabetes;
(4) A medicament for treating or preventing kidney disease.
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