阅读说明：本技术 一种植物甾醇酯微胶囊及其制备方法与应用 (Phytosterol ester microcapsule and preparation method and application thereof ) 是由 孙凤刚 邹胜龙 李志华 潘忠超 于 2019-09-27 设计创作，主要内容包括：本发明属于精细化工领域,具体涉及一种植物甾醇酯微胶囊及其制备方法与应用。本发明以维生素C水溶液为水相,以植物甾醇酯作为油相,辅以乳化剂,制备得到稳定的W/O乳液,然后以该W/O乳液作为芯材,以负电荷聚合物阿拉伯胶、果胶和正电荷聚合物壳聚糖作为壁材,进行复合凝聚反应,得到稳定的植物甾醇酯微胶囊。该微胶囊耐高温、高湿,并具有缓释作用,方法简单,反应温和。(The invention belongs to the field of fine chemical engineering, and particularly relates to a phytosterol ester microcapsule as well as a preparation method and application thereof. The invention takes vitamin C water solution as water phase, takes plant sterol ester as oil phase, is assisted by emulsifier to prepare stable W/O emulsion, then takes the W/O emulsion as core material, takes negative charge polymer Arabic gum, pectin and positive charge polymer chitosan as wall material to carry out complex coacervation reaction, and obtains stable plant sterol ester microcapsule. The microcapsule is resistant to high temperature and high humidity, has a slow release effect, and is simple in method and mild in reaction.)

1. A preparation method of phytosterol ester microcapsules is characterized by comprising the following steps:

(1) taking a vitamin C water solution with the mass fraction of 0.5-5% as a water phase and phytosterol ester as an oil phase, adding the water phase into the oil phase phytosterol ester, then adding an emulsifier, and dispersing at a high speed to obtain a W/O emulsion;

(2) mixing Arabic gum and pectin according to a mass ratio of 1: (3-5) mixing to obtain a mixed colloid; then dissolving the mixed colloid in water to obtain a mixed colloid solution;

(3) slowly adding the W/O emulsion prepared in the step (1) into the mixed colloidal solution under the stirring condition, uniformly mixing, then adding a chitosan acetic acid solution with the mass fraction of 1-2%, and uniformly mixing to obtain a mixed system;

(4) adjusting the pH value of the reaction system in the step (3) to 3.5-4.0, stirring at 25-35 ℃ for reaction for 5-12 h, standing at 0-4 ℃ for 2-4 h, and centrifuging and collecting to obtain a phytosterol ester microcapsule wet capsule;

(5) and (4) further drying the wet plant sterol ester microcapsule prepared in the step (4) to obtain the plant sterol ester microcapsule.

2. A process for the preparation of phytosterol ester microcapsules according to claim 1, wherein:

the mass ratio of the water phase to the oil phase in the step (1) is (4-6): 6.

3. A process for the preparation of phytosterol ester microcapsules according to claim 1, wherein:

the emulsifier in the step (1) is preferably a mixture of lecithin and phytosterol;

the mass ratio of the lecithin to the phytosterol is (2-4): 3.

4. a process for the preparation of phytosterol ester microcapsules according to claim 1, wherein:

the dosage of the emulsifier in the step (1) is 0.5-3% of the mass of the water phase and the oil phase.

5. A process for the preparation of phytosterol ester microcapsules according to claim 1, wherein:

the mass fraction of the mixed colloid in the step (2) is 1-2%.

The mass fraction of chitosan in the chitosan acetic acid solution in the step (3) is 1-2%.

6. A process for the preparation of phytosterol ester microcapsules according to claim 1, wherein:

the molecular weight of the chitosan in the step (3) is 5-15 ten thousand.

7. A process for the preparation of phytosterol ester microcapsules according to claim 1, wherein:

the mass ratio of the mixed colloid and the chitosan in the step (3) is as follows: (3.2-3.8): 1.

8. a process for the preparation of phytosterol ester microcapsules according to claim 1, wherein:

the mass ratio of the chitosan, the mixed colloid and the phytosterol ester in the step (3) is 2: 1.

9. A phytosterol ester microcapsule, which is characterized by being prepared by the preparation method of any one of claims 1-8.

10. Use of phytosterol ester microcapsules according to claim 9 in the fields of medicine, feed and food.

Technical Field

The invention belongs to the field of fine chemical engineering, and particularly relates to a phytosterol ester microcapsule as well as a preparation method and application thereof.

Background

Phytosterols are natural active substances present in plants, structurally similar to animal sterols such as cholesterol, and are found in a wide variety of vegetable oils, nuts, plant seeds, vegetables and fruits. Natural phytosterols are diverse in variety, mainly including beta-sitosterol, stigmasterol, brassicasterol, and campesterol. The phytosterol ester is prepared by esterification reaction of phytosterol and fatty acid, has better fat solubility than free phytosterol, better fat solubility than phytosterol and better blood cholesterol reducing effect. The FDA in the united states has approved the use of "good health" labels for foods supplemented with phytosterols or phytosterol esters, and the FDA makes statements according to research reports that cholesterol lowering efficacy can be achieved with at least 1.3g of phytosterol ester per day.

Phytosterol esters are lipid-soluble substances which are better than phytosterols, but are still difficult to be mixed with water-soluble substances, are difficult to be added into food and medicines uniformly, and are easy to increase in peroxide value and cause oxidative rancidity when exposed to air. These factors contribute to the limitations of the use of phytosterol esters. The application range of the phytosterol ester can be expanded by microencapsulating the phytosterol ester.

The microcapsule technology is a technology for embedding solid, liquid or gas into a functional core-shell structure inclusion compound by using a film-forming material. The prepared inclusion compound is called a microcapsule, the particle size of the microcapsule is usually from several micrometers to thousands of micrometers, wherein, the substance which is wrapped inside is called a core material, also called guest molecules, the coating material which is outside is called a wall material, also called main body molecules, the wall material is generally natural or synthetic polymer material, and the core material can be liquid, solid or gas, and can be a mixture of one or more substances. As a new technology, the microcapsule has been widely applied in the fields of food, chemical industry, agriculture, and the like, and the microencapsulation technology can be classified into a physical method, a chemical method, and a physicochemical method according to the principle. Wherein, the physical method mainly comprises a spray drying method, a fluidized bed coating method, an air suspension method and the like; the chemical methods mainly comprise an in-situ polymerization method, a complex coacervation method, a method for preparing microcapsules by using liposome and the like; the physical and chemical methods mainly include coacervation phase separation, solvent evaporation, and sol-gel embedding.

Disclosure of Invention

In order to overcome the disadvantages and drawbacks of the prior art, the primary object of the present invention is to provide a method for preparing phytosterol ester microcapsules.

The invention also aims to provide the phytosterol ester microcapsule prepared by the preparation method.

Still another object of the present invention is to provide the use of the plant sterol ester microcapsule.

The purpose of the invention is realized by the following technical scheme:

a preparation method of phytosterol ester microcapsules comprises the following steps:

(1) taking a vitamin C water solution with the mass fraction of 0.5-5% as a water phase and phytosterol ester as an oil phase, adding the water phase into the oil phase phytosterol ester, then adding an emulsifier, and dispersing at a high speed to obtain a W/O emulsion;

(2) mixing Arabic gum and pectin according to a mass ratio of 1: (3-5) mixing to obtain a mixed colloid; then dissolving the mixed colloid in water to obtain a mixed colloid solution;

(3) slowly adding the W/O emulsion prepared in the step (1) into the mixed colloidal solution under the stirring condition, uniformly mixing, then adding a chitosan acetic acid solution with the mass fraction of 1-2%, and uniformly mixing to obtain a mixed system;

(4) adjusting the pH value of the reaction system in the step (3) to 3.5-4.0, stirring at 25-35 ℃ for reaction for 5-12 h, standing at 0-4 ℃ for 2-4 h, and centrifuging and collecting to obtain a phytosterol ester microcapsule wet capsule;

(5) further drying the wet plant sterol ester microcapsule prepared in the step (4) to obtain plant sterol ester microcapsules;

the mass ratio of the water phase to the oil phase in the step (1) is preferably (4-6): 6;

the emulsifier in the step (1) is preferably a mixture of lecithin and phytosterol;

the mass ratio of the lecithin to the phytosterol is preferably (2-4): 3;

the dosage of the emulsifier in the step (1) is preferably 0.5-3% of the mass of the water phase and the oil phase;

the condition of high-speed dispersion in the step (1) is preferably 10000-12000 r/min for 4-10 min of dispersion;

the mass fraction of the mixed colloid in the step (2) is 1-2%;

the mass fraction of chitosan in the chitosan acetic acid solution in the step (3) is 1-2%;

the molecular weight of the chitosan in the step (3) is preferably 5-15 ten thousand;

the mass ratio of the mixed colloid and the chitosan in the step (3) is as follows: (3.2-3.8): 1;

the mass ratio of the chitosan and the mixed colloid (namely the wall material) to the phytosterol ester in the step (3) is preferably 2: 1;

a phytosterol ester microcapsule, which is prepared by the preparation method;

the phytosterol ester microcapsule is applied to the fields of medicines, feeds and foods;

vitamin C is an important antioxidant, the property of vitamin C is very unstable, environmental factors such as temperature, pH value, oxygen, metal ions, ultraviolet rays, X rays and the like can affect the stability of vitamin C, therefore, the vitamin C is very easy to lose activity in the processes of processing, transportation, taking out of a cabin and using of granulated feed, phytosterol ester belongs to greasy substances, has better lipid solubility than phytosterol, is still difficult to be mixed with water-soluble substances, is difficult to be uniformly added into food and medicines, and the peroxide value of the phytosterol ester is easy to rise and oxidation rancidity occurs when the phytosterol ester is exposed to air. Based on the water solubility, oxidation resistance, instability and fat solubility and instability of vitamin C, the invention firstly takes water solution as water phase, plant sterol ester as oil phase, emulsifier is assisted, stable W/O emulsion is prepared, then the W/O emulsion is taken as core material, negative charge polymer Arabic gum, pectin and positive charge polymer chitosan are taken as wall material, complex coacervation reaction is carried out, wherein, chitosan is dissolved in dilute acetic acid to generate a large amount of positive charge primary amino groups on molecular chain, pectin and Arabic gum are dissolved in water to form a large amount of negative charge carboxyl groups, the chitosan solution, pectin and Arabic gum can form polyelectrolyte membrane through positive and negative charge attraction, besides, the chitosan and pectin molecules are straight chain structures, Arabic gum molecules are branched, and are further crosslinked in the reaction process, obtaining the stable phytosterol ester microcapsule.

Compared with the prior art, the invention has the following advantages and effects:

(1) the plant sterol ester microcapsule prepared by the method of emulsification, complex coacervation and the like comprises the active components of vitamin C and plant sterol ester, wherein the vitamin C is positioned in the inner core part of the plant sterol ester microcapsule through complex emulsification-complex coacervation, and the stability is extremely high.

(2) The inner core part of the phytosterol ester microcapsule prepared by the invention is vitamin C, and the antioxidant property of the vitamin C can protect the oxidative rancidity of the phytosterol ester.

(3) The middle layer of the phytosterol ester microcapsule prepared by the invention is the phytosterol ester which has fat solubility and can maintain the activity of the vitamin C in the inner core, namely the vitamin C and the phytosterol ester are mutually protective agents.

(4) The outermost layer of the phytosterol ester microcapsule prepared by the invention is a polyelectrolyte composite film formed by chitosan-Arabic gum and chitosan and pectin, so that the phytosterol ester microcapsule further has a protective effect on the inner core vitamin C and the phytosterol ester in the middle layer, and the water solubility of the phytosterol ester is greatly improved.

(5) In the W/O emulsion emulsification process, the invention takes phytosterol and the like as the emulsifier, has good emulsification effect and does not introduce other excessive emulsifiers. In the secondary emulsification process, no additional emulsifier is added, and the wall material additives pectin and Arabic gum can serve as the wall material and the emulsifier simultaneously, so that the emulsification effect is good.

(6) The pectin replaces part of the acacia gum with higher cost, and the cost is reduced while the complex coacervation effect is not influenced.

(7) The phytosterol ester microcapsule prepared by the invention is used for feed addition, has the characteristics of promoting the growth and development of animals, resisting biological oxidation in organisms, improving the quality of meat products and the like, and has the advantages of good stability, high embedding rate, high temperature and high humidity resistance, slow release effect, mild preparation process, high yield and high efficiency.

Drawings

Fig. 1 is a graph showing the results of analyzing the sustained release at 25 c of room temperature of the phytosterol ester microcapsule prepared in example 1.

Detailed Description

The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited thereto.