CN112168850B - Preparation method of hydrophilic seabuckthorn sterol - Google Patents

Preparation method of hydrophilic seabuckthorn sterol Download PDF

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CN112168850B
CN112168850B CN202011078138.5A CN202011078138A CN112168850B CN 112168850 B CN112168850 B CN 112168850B CN 202011078138 A CN202011078138 A CN 202011078138A CN 112168850 B CN112168850 B CN 112168850B
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sterol
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seabuckthorn
hydrophilic
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CN112168850A (en
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张得钧
郭阳
张本印
杨永晶
张永倩
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Qinghai University
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • 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
    • A23L29/015—Inorganic compounds
    • 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
    • A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/206—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
    • A23L29/256—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin from seaweeds, e.g. alginates, agar or carrageenan
    • 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
    • A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/288—Synthetic resins, e.g. polyvinylpyrrolidone
    • 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
    • A23L33/11—Plant sterols or derivatives thereof, e.g. phytosterols
    • 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
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
    • A61K47/32—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds, e.g. carbomers, poly(meth)acrylates, or polyvinyl pyrrolidone
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
    • A61K47/36—Polysaccharides; Derivatives thereof, e.g. gums, starch, alginate, dextrin, hyaluronic acid, chitosan, inulin, agar or pectin
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00—Medicinal preparations characterised by special physical form
    • A61K9/06—Ointments; Bases therefor; Other semi-solid forms, e.g. creams, sticks, gels
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P3/00—Drugs for disorders of the metabolism
    • A61P3/06—Antihyperlipidemics
    • 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 relates to the technical field of extraction and preparation of phytosterol, and particularly relates to a preparation method of hydrophilic seabuckthorn sterol. The method specifically comprises six steps of gel matrix preparation, sterol aqueous emulsion preparation, cross-linking agent preparation and solidification, pellet preparation, drying and drug loading rate and encapsulation rate measurement. The preparation method of the hydrophilic seabuckthorn sterol has simple process steps and easy operation; the requirements of equipment specification and parameter index are low, and the price of the required reagent is low; the sodium alginate-polyvinyl alcohol embedding is utilized, so that the hydrophilicity of sterol can be improved, no toxicity is caused, and the finally obtained drug loading rate and encapsulation rate are high; the method develops a new path for the seabuckthorn sterol in the field of food and medicine, provides an important reference basis for the development of hydrophilic medicines, and has great economic and social benefits.

Description

Preparation method of hydrophilic seabuckthorn sterol
Technical Field
The invention relates to the technical field of extraction and preparation of phytosterol, and particularly relates to a preparation method of hydrophilic seabuckthorn sterol.
Background
Hippophae rhamnoides (Hippophae rhamnoides Lin.) is a plant of Hippophae of Elaeagnaceae, is mainly distributed in Qinghai-Tibet plateau, inner Mongolia desert, loess plateau, etc., and has the characteristics of drought resistance, cold resistance, barren resistance, salt resistance, alkali resistance, etc. Sea buckthorn is rich in various bioactive components, such as phytosterol, flavone, vitamin C and the like. Research shows that the beta-sitosterol contained in the sea buckthorn seed oil has the functions of inhibiting platelet aggregation and resisting inflammation, can also obviously reduce the level of cholesterol in vivo, and has obvious inhibiting effect on the growth of tumors and the diffusion of cancer cells. In addition, the seabuckthorn sterol can promote the body to regulate the immune system, has stronger antioxidation, and is used as a clinical medicament for preventing and treating cardiovascular disorders such as hyperlipidemia, atherosclerosis, palpitation, chest distress, coronary arteriosclerotic heart disease and the like.
The seabuckthorn sterol belongs to a natural active substance with good biocompatibility, takes cyclopentane perhydrophenanthrene as a skeleton, can reduce the content of total cholesterol and the level of low-density lipoprotein cholesterol in serum, has wide application, covers the fields of medicines, foods, cosmetics and the like, and has good market prospect. The sea buckthorn sterol is insoluble in water and has low bioavailability, and the insolubility greatly reduces the application range of the sea buckthorn sterol in the food industry. The research on the preparation method of the hydrophilic phytosterol at home and abroad mainly comprises methods such as nano particles, physical embedding, emulsion and the like. Phytosterol-protein microcapsules: lecithin and monoglyceride are used as an emulsifier, protein is used as a wall material, phytosterol is dissolved in vegetable oil, and finally the product is prepared by drying. The method can increase the peroxide value of the product and remarkably reduce the utilization rate of phytosterol. Nanoemulsion of phytosterols: the use of protein with high hydrophilicity improves much water solubility, but due to the hydrophilicity of the protein, the embedding redissolution is poor, the stability is low, the bioavailability is low, and a large amount of organic reagent is needed in the production process, so that the safety problem exists.
Disclosure of Invention
In order to solve the technical problems, the gel matrix is prepared from the polyvinyl alcohol and the sodium alginate, and the gel matrix is prepared from Span 80: tween80 is used for preparing aqueous emulsion of sterol, anhydrous calcium chloride is used for preparing cross-linking agent, matrix and the aqueous emulsion of sterol are fully stirred to obtain small balls, and the drug loading rate and the encapsulation rate are calculated after freeze drying. Aims to provide a preparation method of hydrophilic seabuckthorn sterol.
The invention relates to a preparation method of hydrophilic seabuckthorn sterol, which adopts the technical scheme that: the method specifically comprises the following steps:
step one, preparing a gel matrix: mixing polyvinyl alcohol and sodium alginate in a ratio of 3: 4, putting the mixture into distilled water of 60-90 mL, fully stirring, and sterilizing at high temperature for 15-20 min to mix and dissolve the mixture for later use;
step two, preparing sterol water emulsion: firstly, pouring 4-6 mL of distilled water into conical flasks respectively for later use, pouring 4-6 mL of olive oil into a beaker for later use, and adding the volumes of the two into 10 mL; then, weighing sterol, adding the sterol into the prepared olive oil according to the material-liquid ratio of 1-2: 2-5, adding Tween80 into the prepared distilled water to fully dissolve the sterol for later use, and adding Span80 into the olive oil with the sterol to fully dissolve the sterol for later use; finally, mixing and emulsifying the aqueous solution of Tween80 and olive oil of sterol dissolved with Span80 to prepare sterol aqueous emulsion, wherein the ratio of Span 80: tween80 ═ 1: 5;
step three, preparing and curing a cross-linking agent: weighing quantitative anhydrous calcium chloride, and preparing into a cross-linking agent for later use; the gel matrix is taken as a carrier, and the prepared calcium chloride solution cross-linking agent is immobilized;
Step four, preparing the pellets: mixing the gel matrix with the sterol aqueous emulsion according to the ratio of 2: 1, fully stirring the mixture in a stirrer at the temperature of between 30 and 37 ℃ and the rotating speed of between 45 and 50r/s to prepare small balls;
step five, drying: filtering the prepared pellets, filtering out the cross-linking solution, washing the pellets with distilled water for 2-3 times, removing the surface calcium chloride solution, and drying;
step six, measuring the drug loading rate and the encapsulation efficiency: accurately weighing appropriate amount of the fine small ball powder, adding anhydrous alcohol, performing ultrasonic treatment to dissolve the medicine, and fixing the volume; filtering, taking the filtrate, diluting by proper times, measuring the absorbance at the wavelength of 548nm, and calculating the concentration of the microsphere loaded sterol, the concentration of the sterol standard product, the microsphere drug loading rate and the encapsulation rate by utilizing a regression equation.
Further, a high-pressure steam sterilization pot is adopted for high-temperature sterilization in the first step, and the temperature of the mould is 110-121 ℃.
Further, the emulsification treatment in the second step adopts a constant-temperature magnetic stirrer.
Furthermore, the stirrer for preparing the small balls in the fourth step adopts a constant-temperature magnetic stirrer, and the prepared small balls are required to have no dissolution phenomenon, no adhesion and uniform balls.
Further, a freeze dryer is adopted for drying in the fifth step.
Compared with the prior art, the invention has the following beneficial effects: the preparation method of the hydrophilic seabuckthorn sterol has simple process steps and easy operation; the requirements of equipment specification and parameter index are low, and the price of the required reagent is low; the sodium alginate-polyvinyl alcohol embedding is utilized, so that the hydrophilicity of sterol can be improved, no toxicity is caused, and the finally obtained drug loading rate and encapsulation rate are high; the method develops a new path for the seabuckthorn sterol in the field of food and medicine, provides an important reference basis for the development of hydrophilic medicines, and has great economic and social benefits.
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FIG. 1 is a process flow diagram of the method of the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The technical scheme of the preparation method of the hydrophilic seabuckthorn sterol comprises the following steps: the method specifically comprises the following steps:
Step one, preparing a gel matrix: mixing polyvinyl alcohol and sodium alginate in a ratio of 3: 4, putting the mixture into 60mL of distilled water, fully stirring, putting the mixture into a high-pressure steam sterilization pot at the temperature of 110 ℃ for sterilization for 20min, and mixing and dissolving the mixture for later use;
step two, preparing sterol aqueous emulsion: firstly, pouring 4mL of distilled water into conical flasks respectively for later use, pouring 6mL of olive oil into a beaker for later use, and adding the volumes of the two into 10 mL; then, weighing sterol, adding the sterol into the prepared olive oil according to the material-liquid ratio of 1-2: 2-5, adding Tween80 into the prepared distilled water to fully dissolve the sterol for later use, and adding Span80 into the olive oil with the sterol to fully dissolve the sterol for later use; and finally, mixing the Tween80 aqueous solution and the olive oil in which the Span80 sterol is dissolved, and emulsifying in a constant-temperature magnetic stirrer to prepare the sterol water emulsion, wherein the ratio of Span 80: tween80 ═ 1: 5;
step three, preparing and curing a cross-linking agent: weighing quantitative anhydrous calcium chloride, and preparing into a cross-linking agent for later use; the gel matrix is taken as a carrier, and the prepared calcium chloride solution cross-linking agent is immobilized;
step four, preparing the pellets: mixing the gel matrix with the sterol aqueous emulsion according to the ratio of 2: 1, fully stirring the mixture in a constant-temperature magnetic stirrer at the rotating speed of 45r/s at the temperature of 30 ℃ to prepare small balls, wherein the prepared small balls are required to have no dissolution phenomenon, no adhesion and uniform balls;
Step five, drying: filtering the prepared pellet, filtering to remove cross-linking solution, washing the pellet with distilled water for 2 times, removing surface calcium chloride solution, and drying with freeze drier;
step six, measuring the drug loading rate and the encapsulation efficiency: accurately weighing appropriate amount of the fine small ball powder, adding anhydrous alcohol, performing ultrasonic treatment to dissolve the medicine, and fixing the volume; filtering, taking the filtrate, diluting by proper times, measuring the absorbance at 548nm wavelength, and calculating by using a regression equation that the concentration of the microsphere loaded sterol is 31.8mg/mL, the concentration of the sterol standard product is 73.9mg/mL, the microsphere loaded drug rate is 31.8% and the encapsulation rate is 15.9%.
Example 2
The technical scheme of the preparation method of the hydrophilic seabuckthorn sterol comprises the following steps: the method specifically comprises the following steps:
step one, preparing a gel matrix: mixing polyvinyl alcohol and sodium alginate in a ratio of 3: 4, putting the mixture into 90mL of distilled water, fully stirring, putting the mixture into a high-pressure steam sterilization pot at the temperature of 121 ℃ for sterilization for 15min, and mixing and dissolving the mixture for later use;
step two, preparing sterol aqueous emulsion: firstly, pouring 5mL of distilled water into conical flasks for later use, pouring 5mL of olive oil into a beaker for later use, and adding the volumes of the two into 10 mL; then, weighing sterol, adding the sterol into the prepared olive oil according to the material-liquid ratio of 1-2: 2-5, adding Tween80 into the prepared distilled water to fully dissolve the sterol for later use, and adding Span80 into the olive oil with the sterol to fully dissolve the sterol for later use; and finally, mixing the Tween80 aqueous solution and the olive oil in which the Span80 sterol is dissolved, and emulsifying in a constant-temperature magnetic stirrer to prepare the sterol water emulsion, wherein the ratio of Span 80: tween80 ═ 1: 5;
Step three, preparing and curing a cross-linking agent: weighing quantitative anhydrous calcium chloride, and preparing into a cross-linking agent for later use; the gel matrix is taken as a carrier, and the prepared calcium chloride solution cross-linking agent is immobilized;
step four, preparing pellets: mixing the gel matrix with the sterol aqueous emulsion according to the ratio of 2: 1, fully stirring the mixture in a constant-temperature magnetic stirrer at the rotating speed of 50r/s at 37 ℃ to prepare small balls, wherein the prepared small balls are required to have no dissolution phenomenon, no adhesion and uniform balls;
step five, drying: filtering the prepared pellet, filtering to remove cross-linking solution, washing the pellet with distilled water for 3 times, removing surface calcium chloride solution, and drying with freeze drier;
step six, measuring the drug loading rate and the encapsulation efficiency: accurately weighing appropriate amount of the fine small ball powder, adding appropriate amount of anhydrous alcohol, performing ultrasonic treatment to dissolve the medicine, and fixing the volume; filtering, taking the filtrate, diluting by proper times, measuring the absorbance at 548nm wavelength, and calculating by using a regression equation that the concentration of the microsphere loaded sterol is 33.2mg/mL, the concentration of the sterol standard product is 77.1mg/mL, the microsphere loaded drug rate is 33.2%, and the encapsulation rate is 16.6%.
Example 3
The technical scheme of the preparation method of the hydrophilic seabuckthorn sterol comprises the following steps: the method specifically comprises the following steps:
Step one, preparing a gel matrix: mixing polyvinyl alcohol and sodium alginate in a ratio of 3: 4, putting the mixture into 80mL of distilled water, fully stirring, putting the mixture into a high-pressure steam sterilization pot at the temperature of 115 ℃ for sterilization for 18min, and mixing and dissolving the mixture for later use;
step two, preparing sterol water emulsion: firstly, pouring 6mL of distilled water into conical flasks for later use, pouring 4mL of olive oil into a beaker for later use, and adding the volumes of the two into 10 mL; then, weighing sterol, adding the sterol into the prepared olive oil according to the material-liquid ratio of 1-2: 2-5, adding Tween80 into the prepared distilled water to fully dissolve the sterol for later use, and adding Span80 into the olive oil with the sterol to fully dissolve the sterol for later use; and finally, mixing the Tween80 aqueous solution and the olive oil in which the Span80 is dissolved, and emulsifying in a constant-temperature magnetic stirrer to prepare the sterol aqueous emulsion, wherein the ratio of Span 80: tween80 ═ 1: 5;
step three, preparing and curing a cross-linking agent: weighing quantitative anhydrous calcium chloride, and preparing into a cross-linking agent for later use; the gel matrix is taken as a carrier, and the prepared calcium chloride solution cross-linking agent is immobilized;
step four, preparing the pellets: mixing the gel matrix with the sterol aqueous emulsion according to the ratio of 2: 1, fully stirring the mixture in a constant-temperature magnetic stirrer at the rotating speed of 48r/s at the temperature of 35 ℃ to prepare small balls, wherein the prepared small balls are required to have no dissolution phenomenon, no adhesion and uniform balls;
Step five, drying: filtering the prepared pellet, filtering to remove cross-linking solution, washing the pellet with distilled water for 3 times, removing surface calcium chloride solution, and drying with a freeze dryer;
step six, measuring the drug loading rate and the encapsulation efficiency: accurately weighing appropriate amount of the fine small ball powder, adding anhydrous alcohol, performing ultrasonic treatment to dissolve the medicine, and fixing the volume; filtering, taking the filtrate, diluting by proper times, measuring the absorbance at 548nm wavelength, and calculating by using a regression equation that the concentration of the microsphere loaded sterol is 33.6mg/mL, the concentration of the sterol standard product is 78.1mg/mL, the microsphere loaded drug rate is 33.6%, and the encapsulation rate is 16.8%.
Example 4
Optimization experiment of preparation method of hydrophilic seabuckthorn sterol globules
1. Effect of different embedding agent ratios on pellet immobilization
Mixing the raw materials in a ratio of 1: 2. 2: 3. 3: 4, weighing Sodium Alginate (SA) and polyvinyl alcohol (PVA) according to three proportions, placing the Sodium Alginate (SA) and the PVA into the same amount of sterile water, fully stirring the mixture, putting the mixture into a high-pressure steam sterilization pot (the temperature is 121 ℃ and the time is 20min) to be mixed and dissolved to be used as a gel matrix for preparing the small balls, and then cooling the matrix to prepare the small balls and comparing the balling effect (see table 1 for details).
TABLE 1 conditions of pellets after immobilization with different embedding agent ratios
Figure BDA0002716914670000081
As a result, Sodium Alginate (SA): polyvinyl alcohol (PVA) ═ 3: the pellet prepared by the method 4 has good elasticity, is not easy to break, has no tailing, is not easy to generate adhesion condition, and has good balling effect. Thus, Sodium Alginate (SA) was determined: polyvinyl alcohol (PVA) ═ 3: 4 is the optimum ratio.
2. Effect of different concentrations of gel matrix on pellet immobilization
Weighing distilled water by three volumes of 30, 60 and 90, wherein the weight ratio of Sodium Alginate (SA) to polyvinyl alcohol (PVA) is 3: 4 weighing the medicines for standby, preparing gel matrixes with different concentrations, and cooling the matrixes to prepare balls (see table 2 for details).
TABLE 2 Effect of different concentrations of gel matrix on pellet immobilization
Figure BDA0002716914670000082
Figure BDA0002716914670000091
As a result, Sodium Alginate (SA): polyvinyl alcohol (PVA) ═ 3: 4, when the distilled water is 60-90 mL, the prepared gel matrix can be prepared into small balls, and the ball preparation effect is good. Sodium Alginate (SA) was thus determined: polyvinyl alcohol (PVA) ═ 3: and 4, distilled water is 60-90 mL, and is in a proper proportion (see table 2 for details).
3. Selection of sterol dissolving solvent
0.2g of sterol is weighed and respectively added into 5mL of absolute ethyl alcohol, DMSO, dichloromethane, olive oil and distilled water, the mixture is fully stirred and then subjected to ultrasonic dissolution promotion and is mixed with a substrate for observation, and a proper sterol solvent is further selected, so that the absolute ethyl alcohol, the DMSO, the dichloromethane and the like which are used as dissolved sterol solvents react with the substrate, and the distilled water has too low solubility, so that the olive oil is selected as a solvent (see table 3 for details).
TABLE 3 dissolution Effect of different solvents on sterols
Figure BDA0002716914670000092
4. Span80 of different ratios: effect of Tween80 on emulsification Effect
In the preparation of the emulsion, 4mL, 5mL, 6mL of H were measured in high-precision measuring cylinders2O, 6mL, 5mL and 4mL of olive oil, the volume sum of the two is just 10mL, the two are respectively poured into a prepared conical flask and a beaker slowly, and 2g of sterol is added into the olive oil; selecting emulsifier according to HLB value, adding high HLB value Tween80, and adding H2In O, adding Span80 into olive oil; and then shaking the container to completely dissolve the emulsifier in distilled water or olive oil, mixing the distilled water solution dissolved with Tween80 with the olive oil dissolved with Span80 sterol, and emulsifying by using a constant-temperature magnetic stirrer, wherein the ratio of Span 80: tween80 ═ 1: the best emulsification was found at 5 (see table 4 for details).
Table 4 different ratios of Span 80: effect of Tween80 on emulsification Effect
Figure BDA0002716914670000101
5. Influence of different gel matrix and aqueous emulsion ratios on inclusion effect
Taking three clean conical flasks, mixing the gel matrix with the sterol water emulsion according to the weight ratio of 1: 1. 1: 2. 2: 1, stirring the mixture fully by a constant-temperature magnetic stirrer at 37 ℃ and a rotating speed of 50r/s, observing the phenomenon, and selecting the optimal ratio of the matrix to the aqueous emulsion. According to the observation phenomenon, the optimal ratio of the gel matrix to the sterol water emulsion is 2: 1 (see table 5 for details).
TABLE 5 dissolution Effect of different solvents on sterols
Figure BDA0002716914670000102
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (5)

1. A preparation method of hydrophilic seabuckthorn sterol is characterized by comprising the following steps:
step one, preparing a gel matrix: mixing polyvinyl alcohol and sodium alginate in a ratio of 3: 4, putting the mixture into distilled water of 60-90 mL, fully stirring, and sterilizing at high temperature for 15-20 min to mix and dissolve the mixture for later use;
step two, preparing sterol aqueous emulsion: firstly, pouring 4-6 mL of distilled water into conical flasks respectively for later use, pouring 4-6 mL of olive oil into a beaker for later use, and adding the volumes of the two into 10 mL; then, weighing sterol, adding the sterol into the prepared olive oil according to the material-liquid ratio of 1-2: 2-5, adding Tween80 into the prepared distilled water to fully dissolve the sterol for later use, and adding Span80 into the olive oil with the sterol to fully dissolve the sterol for later use; finally, mixing and emulsifying the aqueous solution of Tween80 and olive oil of sterol dissolved with Span80 to prepare sterol aqueous emulsion, wherein the ratio of Span 80: tween80 ═ 1: 5;
Step three, preparing and curing a cross-linking agent: weighing a certain amount of anhydrous calcium chloride, and preparing into a cross-linking agent for later use; the gel matrix is taken as a carrier, and the prepared calcium chloride solution cross-linking agent is immobilized;
step four, preparing the pellets: mixing the gel matrix with the sterol aqueous emulsion according to the ratio of 2: 1, fully stirring the mixture in a stirrer at the temperature of between 30 and 37 ℃ and the rotating speed of between 45 and 50r/s to prepare small balls;
step five, drying: filtering the prepared pellets, filtering out the cross-linking solution, washing the pellets with distilled water for 2-3 times, removing the surface calcium chloride solution, and drying;
step six, measuring the drug loading rate and the encapsulation efficiency: accurately weighing appropriate amount of the fine small ball powder, adding anhydrous alcohol, performing ultrasonic treatment to dissolve the medicine, and fixing the volume; filtering, taking the filtrate, diluting by proper times, measuring the absorbance at the wavelength of 548nm, and calculating the concentration of the microsphere loaded sterol, the concentration of the sterol standard product, the microsphere drug loading rate and the encapsulation rate by utilizing a regression equation.
2. The method for preparing hydrophilic seabuckthorn sterol according to claim 1, wherein the high-temperature sterilization in the first step adopts a high-pressure steam sterilization pot, and the sterilization temperature is 110-121 ℃.
3. The method for preparing hydrophilic seabuckthorn sterols according to claim 1, wherein a constant temperature magnetic stirrer is used for emulsification treatment in the second step.
4. The method for preparing hydrophilic seabuckthorn sterols according to claim 1, wherein a constant temperature magnetic stirrer is used as a stirrer for preparing the small balls in the fourth step, and the prepared small balls are required to have no dissolution phenomenon, no adhesion and uniform spheres.
5. The method according to claim 1, wherein a freeze dryer is used for drying in the fifth step.
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