阅读说明：本技术 一种叶黄素酯和水溶型叶黄素酯微胶囊及其制备方法 (Lutein ester and water-soluble lutein ester microcapsule and preparation method thereof ) 是由 李宏龙 徐小松 文雁君 李林正 章文晋 於春峰 夏慧婷 于 2020-06-29 设计创作，主要内容包括：本申请公开了一种叶黄素酯和水溶型叶黄素酯微胶囊及其制备方法。本发明从万寿菊颗粒中提取叶黄素酯,经过浓缩、洗涤、脱残后得到叶黄素酯,再将叶黄素酯通过采用二次包埋法工艺,制备得到叶黄素酯微胶囊。本发明中叶黄素酯为从万寿菊颗粒中提取,原材料经济易得,没有经过分离提纯,保留了万寿菊颗粒的部分药用价值,增加了叶黄素酯的保健功效,同时采用二次包埋法还可以使得制备得到的胶囊更稳定、易存放,适用在于食品、医药等领域。并且有效解决了现有技术中对于提取设备要求较高的技术问题,进而实现了设备要求低,工艺简单,生产成本大幅度降低的技术效果。(The application discloses lutein ester and water-soluble lutein ester microcapsules and a preparation method thereof. The lutein ester microcapsule is prepared by extracting the lutein ester from marigold particles, concentrating, washing and removing residues to obtain the lutein ester, and then adopting a secondary embedding method process to prepare the lutein ester microcapsule. The lutein ester is extracted from marigold particles, raw materials are economical and easy to obtain, separation and purification are not carried out, partial medicinal value of the marigold particles is reserved, the health-care effect of the lutein ester is improved, and meanwhile, the capsule prepared by adopting a secondary embedding method is more stable and easy to store and is suitable for the fields of food, medicine and the like. And the technical problem that the requirement on extraction equipment is high in the prior art is effectively solved, and the technical effects of low equipment requirement, simple process and great reduction of production cost are further realized.)

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

taking marigold particles, then extracting the dried marigold particles by using a solvent until the extracted solvent is colorless, concentrating the recovered solvent, washing by using a detergent, and separating the detergent to obtain the lutein ester.

2. The method for preparing lutein ester according to claim 1, wherein the solvent is one of n-hexane, acetone, butanone, ethyl acetate and propyl acetate; the detergent is formed by mixing one or any two of ethanol, ethylene glycol, propylene glycol and isopropanol in any proportion, and the washing times are 2-13 times.

3. The method of claim 1 or 2, wherein the lutein ester is prepared in a concentration of 45-70%.

4. A process for the preparation of a lutein ester according to claim 1 or 2, characterized by comprising the following steps: weighing 100g of marigold flower particles, adding into a 2L round-bottom flask, adding 1.5L of acetone, stirring in a water bath at 65 ℃, carrying out heat preservation and reflux, mixing pure ethyl acetate with the marigold flower particles to extract lutein esters and other fat-soluble substances until the refluxed ethyl acetate is colorless, namely completely extracting, recovering the ethyl acetate to obtain a lutein ester crude extract, washing the crude extract with ethanol for 13 times, carrying out vacuum heating to recover a washing agent, adding a small amount of antioxidant, and mixing to obtain the lutein esters.

5. The water-soluble lutein ester microcapsule is characterized by comprising the following raw materials in parts by weight: 1 part of lutein ester, 0.03-2.0 parts of oil phase antioxidant, 1-10 parts of vegetable oil, 1-50 parts of wall material, 0.1-8 parts of emulsifier, 0.02-2.0 parts of water phase antioxidant, 0.2-50 parts of water phase filler and 10-200 parts of water.

6. The method of preparing a lutein ester microcapsule according to claim 5, wherein the preparation method comprises the following steps:

(1) mixing lutein ester, vegetable oil and oil phase antioxidant, heating in oil bath to dissolve uniformly to obtain oil phase, adding wall material, emulsifier, water phase antioxidant and water phase filler into water, heating and dissolving sufficiently to obtain water phase;

(2) slowly adding the oil phase into the water phase under the action of high-speed shearing, uniformly mixing, and homogenizing by a high-pressure homogenizer to obtain lutein ester emulsion;

(3) carrying out secondary embedding and drying on the homogenized lutein ester emulsion to obtain a lutein ester microcapsule semi-finished product;

(4) and (3) curing the lutein ester microcapsule semi-finished product to obtain a lutein ester microcapsule finished product.

7. The process for preparing lutein ester microcapsule according to claim 6,

in the step (1), the dissolving temperature of the oil phase is 70-135 ℃, and the dissolving temperature of the wall material is 60-85 ℃;

in the step (2), the shearing speed is 4000-10000 rpm, and the homogenizing pressure is 20-60 Mpa;

in the step (3), the air inlet temperature of the secondary embedding drying method is 60-120 ℃, and the feeding speed is 10-90 ml per minute;

in the step (4), the curing temperature of the lutein ester microcapsule is-18-120 ℃, and the curing time is 30 minutes-24 hours.

8. The method of claim 7, wherein the oil-phase antioxidant is vitamin E.

9. The method for preparing lutein ester microcapsule according to claim 7, wherein the vegetable oil is any one or a mixture of any two of soybean oil, corn germ oil and perilla oil.

10. The method for preparing lutein ester microcapsule according to claim 7, wherein the wall material is sugar or vegetable gum; wherein the saccharide comprises modified starch, maltodextrin or cyclodextrin, and the vegetable gum is acacia, sesbania gum or guar gum; the emulsifier is a mixture of any two or any three of sucrose fatty acid ester, modified soybean phospholipid, monopalmitate and sodium stearoyl lactate; the water-phase filling agent is one or a mixture of any two of white granulated sugar, glucose syrup and malto-oligosaccharide.

Technical Field

The invention belongs to the technical field of deep processing of bioactive substances, and particularly relates to a method for extracting lutein ester and a method for preparing a water-soluble lutein ester microcapsule.

Background

Tagetes erecta (Tagetes erecta L) native to Mexico. The flower bed is distributed in various places in China, can grow in the area with the altitude of 1150-1480 meters, has large flowers and long flowering period, is also commonly used for flower bed scenery, and has the following medicinal value: clearing away heat and toxic materials, eliminating phlegm, and relieving cough; it has fragrance and can be used as aromatic; has been used as bacteriostatic, sedative and antispasmodic. It is a congeneric plant, Tagetesninuta (T. glanduliflora), containing volatile oil, and has tranquilizing, blood pressure lowering, bronchus dilating, spasmolytic and antiinflammatory effects.

The lutein ester is carotenoid fatty acid ester, has a chemical name of lutein dipalmitate, is easy to dissolve in an organic solvent, is widely present in corn, cabbage, marigold and other plants, and is most abundant in marigold. The lutein ester is a main component substance of human retina and macula lutea areas, has strong oxidation resistance, has multiple effects of preventing oxidative damage of free radicals to eyes, improving eye microcirculation, preventing senile cataract, protecting retina, preventing optic atrophy and the like, and must be taken from food.

The lutein ester is a compound formed by lutein and one molecule or two molecules of fatty acid, has stronger stability than the lutein, and is greatly damaged only by factors such as high temperature, strong acid, oxygen and the like; lutein ester contains fatty acid group, can be naturally hydrolyzed into free lutein in human body, is easy to absorb, and has bioavailability much higher than lutein crystal, document No. 12 in 2008 of 26 month 5 (public notice of health department 2008): the national ministry of health establishes that lutein esters are approved as new resource food functional raw materials, and lutein health products in the current market also mostly use lutein esters as main functional raw materials.

The microencapsulation technology is a pharmacological means for effectively improving the stability and solubility of a drug, a core material is wrapped in a capsule formed by a tiny wall material, active ingredients of the core material are kept from being influenced by external adverse factors, the storage time of the core material is prolonged, and the release of the core material is controlled.

However, the inventor of the present application finds that the above-mentioned technology has at least the following technical problems in implementing the embodiments of the present application:

(1) in the prior art, the process of microencapsulation by using the high-purity lutein ester crystal has high requirements on equipment and needs special complex refining equipment, thereby greatly improving the production cost;

(2) in the prior art, high-purity lutein ester crystals need to be utilized, but the higher the purity of the lutein ester crystals is, the higher the requirements on transportation and storage conditions are, and the production cost is further increased.

How to reduce the production cost becomes a hot spot for those skilled in the art to study.

Disclosure of Invention

In order to overcome the defect of overhigh cost when lutein ester microcapsule powder with different specifications is massively produced, the embodiment of the application provides a method for extracting lutein ester and preparing lutein ester microcapsules. In the invention, lutein ester is extracted from marigold particles, then the lutein ester is obtained after concentration, washing and residue removal, and the lutein ester microcapsule is prepared by a series of processes. The lutein ester is extracted from marigold particles, raw materials are economical and easy to obtain, separation and purification are not carried out, partial medicinal value of the marigold particles is reserved, the health-care effect of the lutein ester is improved, and meanwhile, the capsule prepared by adopting a secondary embedding method is more stable and easy to store and is suitable for the fields of food, medicine and the like.

The technical scheme adopted by the embodiment of the application for solving the technical problem is as follows:

a method for extracting lutein ester, wherein the method comprises the following steps: taking marigold particles, then extracting the dried marigold particles by using a solvent until the extracted solvent is colorless, concentrating the recovered solvent, washing by using a detergent, and separating the detergent to obtain the lutein ester.

Preferably, the solvent is one of n-hexane, acetone, butanone, ethyl acetate and propyl acetate, and the partial solvent has high solubility to lutein ester and is convenient and easy to obtain; the detergent is one or two of ethanol, ethylene glycol, propylene glycol and isopropanol in any proportion, the extracted mixture contains fatty acid, ketone, ketene, glycoside and other polar micromolecules, and the part of the detergent uses a polar benign solvent, so that the requirements of better washing, convenient operation and the like can be met. The washing times are 2-9 times; the prepared lutein ester has a concentration of 45-70%.

The method for preparing the water-soluble lutein ester microcapsule by using the lutein ester comprises the following components: 1 part of lutein ester, 0.03-0.8 part of oil phase antioxidant, 1-8 parts of vegetable oil, 1-30 parts of wall material, 0.1-8 parts of emulsifier, 0.02-0.8 part of water phase antioxidant, 0.2-30 parts of water phase filler and 10-200 parts of water.

Preferably, the method comprises the following steps:

(1) mixing lutein ester, vegetable oil and oil phase antioxidant, heating in oil bath to dissolve uniformly to obtain oil phase, adding wall material, emulsifier, water phase antioxidant and water phase filler into water, heating and dissolving sufficiently to obtain water phase;

(2) slowly adding the oil phase into the water phase under the action of high-speed shearing, uniformly mixing, and homogenizing by a high-pressure homogenizer to obtain lutein ester emulsion;

(3) carrying out secondary embedding and drying on the homogenized lutein ester emulsion to obtain a lutein ester microcapsule semi-finished product;

(4) and (3) curing the lutein ester microcapsule semi-finished product to obtain a lutein ester microcapsule finished product.

Preferably, in the step (1), the oil phase dissolution temperature is 70-135 ℃, the wall material dissolution temperature is 60-85 ℃, the lutein ester with too low temperature cannot be completely dissolved (molecularly), cannot be embedded by the wall material during emulsification, and can float on the liquid level in oil state, so that the product quality is affected, the higher the temperature is, the faster the lutein ester is lost, and the product content is insufficient, and the research of the applicant finds that a better effect can be achieved under the temperature condition.

In the step (2), the shearing speed is 4000-10000 rpm, and the homogenizing pressure is 20-60 Mpa; the dissolved core material and the water phase wall material are quickly combined, the wall material wraps the core material under the action of high shearing force, a uniform microcapsule form is obtained, and a stable oil-in-water emulsification system is achieved. The core material and the wall material can exist in a semi-embedding state at low speed, the speed is high, the formed microcapsule particles can be damaged, the core material can be peeled off from the wall material, and emulsion breaking is carried out.

In the step (3), the air inlet temperature of the secondary embedding drying method is 60-120 ℃, and the feeding speed is 10-90 ml per minute;

in the step (4), the curing temperature of the lutein ester microcapsule is-18-120 ℃, and the curing time is 30 minutes-24 hours.

Preferably, the oil-phase antioxidant is natural vitamin E, and the natural vitamin E can slow down the oxidation of lutein ester, reduce heat loss and prolong shelf life.

Preferably, the vegetable oil is one or a mixture of two of soybean oil, corn germ oil and perilla oil, and the vegetable oil is used to facilitate the dissolving of lutein ester.

Preferably, the wall material is sugar or vegetable gum, and the wall material is a film coating necessary for the microcapsule; wherein the saccharide comprises modified starch, maltodextrin or cyclodextrin, and the vegetable gum is acacia gum, sesbania gum or guar gum.

Preferably, the emulsifier is a mixture of any two or any three of sucrose fatty acid ester, modified soybean phospholipid, monopalmitate and sodium stearoyl lactylate, can stabilize the emulsion and enhance the emulsifying (embedding) capacity of the wall material,

preferably, the aqueous filler is one or a mixture of any two of white granulated sugar, glucose syrup and malto-oligosaccharide, so that the stability of the emulsion can be enhanced, and the risk of emulsion breaking of the emulsion can be reduced.

Compared with the prior art, the invention has the advantages that:

1. due to the adoption of the technical means of directly extracting lutein ester from marigold particles, the technical problem of high requirement on extraction equipment in the prior art is effectively solved, and the technical effects of low equipment requirement and simple process are further realized.

2. The technical means of directly extracting the lutein ester from the marigold particles is adopted, so the technical problem of high cost of preparing the lutein ester in the prior art is effectively solved, the marigold particles are easy to store, the lutein ester after production can directly enter a preparation workshop section through a pipeline after being qualified in detection, the microencapsulated particles are obtained, the yield is not influenced, the product quality is not obviously different from that of pure lutein ester products, and the cost can be greatly reduced.

3. The technical means of directly extracting the lutein ester from the marigold particles is adopted, so that the problem that the transportation and storage conditions of the lutein ester with higher purity in the prior art are higher in requirement is effectively solved, the content of the obtained lutein ester can be controlled by the method, the lutein ester does not need to be further purified when a low-content (0.5-5%) lutein ester microcapsule product is developed, and only a proper range is required to be controlled so as to facilitate the preparation operation.

Detailed Description

The embodiment of the application provides a method for extracting lutein ester and preparing lutein ester microcapsules, and solves the problem that the cost is too high when lutein ester microcapsule powder with different specifications is produced in large-scale production in the prior art.

Firstly, preparing lutein ester: