阅读说明：本技术 一种罗布麻花甾醇类提取物及其制备方法与应用 (Apocynum venetum sterol extract 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：本发明属于植物有效成分提取领域,具体涉及一种罗布麻花甾醇类提取物及其制备方法与应用。本发明以罗布麻花为原料,采用溶剂提取的方式获得含有罗布麻花甾醇的提取液,提取液不采用浓缩的方式采用低温结晶的形式使得提取液中的甾醇结晶析出,一方面操作更为简单,另一方面,过滤后的滤液可直接循环使用,且更为环保安全,避免了有机溶剂的挥发。低温结晶后进一步对粗提取物进行分子蒸馏,使得甾醇进一步富集,去除其他杂质。制得的罗布麻花甾醇类提取物可应用于饲料添加。(The invention belongs to the field of extraction of effective components of plants, and particularly relates to an apocynum venetum sterol extract and a preparation method and application thereof. The method takes the apocynum venetum as a raw material, adopts a solvent extraction mode to obtain the extract containing the apocynum venetum sterol, and adopts a low-temperature crystallization mode to separate out the sterol crystals in the extract without adopting a concentration mode, so that on one hand, the operation is simpler, on the other hand, the filtered filtrate can be directly recycled, the method is more environment-friendly and safe, and the volatilization of an organic solvent is avoided. And after low-temperature crystallization, performing molecular distillation on the crude extract to further enrich the sterol and remove other impurities. The prepared apocynum venetum sterol extract can be applied to feed additives.)

1. A preparation method of an apocynum venetum sterol extract is characterized by comprising the following steps:

(1) drying and crushing the dogbane fried dough twists, and sieving to obtain coarse powder of the dogbane fried dough twists;

(2) mixing the coarse powder of the apocynum venetum prepared in the step (1) with an organic solvent aqueous solution, and extracting for 3-4 times at 45-60 ℃ for 3-5 hours each time; filtering and combining the filtrate;

(3) slowly cooling the filtrate prepared in the step (2) to 10-15 ℃, preserving heat for 8-15h, and filtering; repeating the above operations for 2-3 times, mixing the filtrates, wherein the filtrate is herba Apocyni Veneti sterols crude extract, and the filtrate is circulated to step (2) and used as extraction reagent for recycling;

(4) and (4) carrying out molecular distillation on the apocynum venetum sterol crude extract prepared in the step (4) to obtain an apocynum venetum sterol extract.

2. The method of preparing an apocynum venetum sterol extract according to claim 1, wherein the apocynum venetum sterol extract comprises:

drying the apocynum venetum flowers in the step (1) at the temperature of 20-40 ℃ to constant weight;

the sieving in the step (1) is to sieve by a sieve of 10-60 meshes.

3. The method of preparing an apocynum venetum sterol extract according to claim 1, wherein the apocynum venetum sterol extract comprises:

the organic solvent in the step (2) is at least one of ethyl acetate, ethanol and isopropanol.

4. The method of preparing an apocynum venetum sterol extract according to claim 1, wherein the apocynum venetum sterol extract comprises:

the organic solvent in the step (2) is preferably a mixture of ethyl acetate and ethanol;

the volume ratio of the ethyl acetate to the ethanol is 1-3 (2-5).

5. The method of preparing an apocynum venetum sterol extract according to claim 1, wherein the apocynum venetum sterol extract comprises:

the volume fraction of water in the organic solvent aqueous solution in the step (2) is 5-25%.

6. The method of preparing an apocynum venetum sterol extract according to claim 1, wherein the apocynum venetum sterol extract comprises:

the cooling speed in the step (3) is 1-3 ℃/min.

7. The method of preparing an apocynum venetum sterol extract according to claim 1, wherein the apocynum venetum sterol extract comprises:

the conditions of the molecular distillation in the step (4) are as follows:

the distillation temperature is controlled to be 200-.

8. An apocynum venetum sterol extract characterized by being prepared by the preparation method of any one of claims 1 to 7.

9. Use of an apocynum venetum sterol extract according to claim 8 in the field of feed additive preparation.

10. The use of an apocynum venetum sterol extract according to claim 9 in the field of feed additive preparation, characterized in that:

the additive amount of the apocynum venetum sterol extract in the feed is as follows: 50-200 g/ton of poultry feed, 250 g/ton of pig feed and 250 g/ton of aquatic feed.

Technical Field

The invention belongs to the field of extraction of effective components of plants, and particularly relates to an apocynum venetum sterol extract and a preparation method and application thereof.

Background

Phytosterols are a class of steroids in nature and belong to the class of saturated (or unsaturated) secondary alcohols. The basic skeleton of the sterol molecule is cyclopentane polyhydrophenanthrene nucleus, which consists of three six-membered rings and one five-membered ring, a hydroxyl group is located at position C3, a side chain consisting of more than 7 carbon atoms is located at position C17, and a methyl group is located at each of positions C10 and C13. With the variation of the ring structure and side chains, sterols form a wide variety of derivatives in nature. Plant sterols can be classified into Free Sterol (FS), sterol fatty acid ester (SE), Sterol Glycoside (SG), and ester Acyl Sterol Glycoside (ASG) according to different derivative groups at C3; plant sterols can be classified into three forms, 4-methyl-free sterols, 4-monomethyl sterols, and 4-dimethyl sterols, depending on the number of methyl groups attached at position C4; plant sterols can be classified into sterols and stanols according to the degree of saturation of the carbon-carbon double bond on the sterol ring. Phytosterols are essential components for stabilizing plant cell membranes, and are widely distributed in vegetable oils, seeds, nuts, vegetables and fruits, similar to the role of cholesterol in the body of animals. More than 100 phytosterols have been identified, with β -sitosterol, stigmasterol and campesterol being the most abundant.

The phytosterol has good effects of resisting oxidation, reducing blood fat, diminishing inflammation, reducing fever, resisting cancer, protecting skin and beautifying, and is widely applied to the fields of food, health care products, medicines, cosmetics and the like. Phytosterols may also be used as precursors for the synthesis of steroidal hormonal drugs. At present, the phytosterol is mainly derived from vegetable oil refining leftovers, particularly deodorized distillates. The main components of the deodorized distillate are natural vitamin E (1-20%), phytosterol (10-30%), free fatty acid (30-60%), glyceride (10-20%), volatile matters (aldehyde, ketone and hydrocarbon) obtained by oxide decomposition, and the like. The grease deodorized distillate reported in the present study mainly includes soybean oil deodorized distillate, rapeseed oil deodorized distillate, cottonseed oil deodorized distillate and palm oil deodorized distillate. The soybean oil deodorized distillate and the rapeseed oil deodorized distillate contain more vitamin E and phytosterol, and have higher economic value. Although the deodorized distillate is a good raw material for extracting the phytosterol and the vitamin E, the current method for industrially producing and extracting the sterol only adopts a methyl esterification-molecular distillation method, and the production principle of the methyl esterification-molecular distillation method is that concentrated sulfuric acid is used as a catalyst to carry out methyl esterification on fatty acid into fatty acid methyl ester with low boiling point, and then the sterol is extracted from the deodorized distillate through molecular distillation and crystallization. The method has the disadvantages of long flow, multiple operation steps, low purity and yield of the product and high cost; the use of large amounts of concentrated sulfuric acid, sodium hydroxide, methanol, corrosion of equipment, environmental pollution, and, more importantly, the phytosterols extracted from the deodorized distillate may contain harmful components, directly limiting the application of the phytosterols from this source.

Disclosure of Invention

In order to overcome the defects and shortcomings of the prior art, the invention mainly aims to provide a preparation method of an apocynum venetum sterol extract.

The invention also aims to provide the apocynum venetum sterol extract prepared by the preparation method.

The invention also aims to provide application of the apocynum venetum sterol extract.

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

a method for preparing an apocynum venetum sterol extract comprises the following steps:

(1) drying and crushing the dogbane fried dough twists, and sieving to obtain coarse powder of the dogbane fried dough twists;

(2) mixing the coarse powder of the apocynum venetum prepared in the step (1) with an organic solvent aqueous solution, and extracting for 3-4 times at 45-60 ℃ for 3-5 hours each time; filtering and combining the filtrate;

(3) slowly cooling the filtrate prepared in the step (2) to 10-15 ℃, preserving heat for 8-15h, and filtering; repeating the above operations for 2-3 times, mixing the filtrates, wherein the filtrate is herba Apocyni Veneti sterols crude extract, and the filtrate is circulated to step (2) and used as extraction reagent for recycling;

(4) carrying out molecular distillation on the apocynum venetum sterol crude extract prepared in the step (4) to obtain an apocynum venetum sterol extract;

preferably, the apocynum venetum in the step (1) is dried to constant weight at the temperature of 20-50 ℃;

the sieving in the step (1) is preferably carried out by a sieve of 10-60 meshes;

the organic solvent in the step (2) is preferably at least one of ethyl acetate, ethanol and isopropanol;

the organic solvent in the step (2) is preferably a mixture of ethyl acetate and ethanol;

the volume ratio of the ethyl acetate to the ethanol is preferably (1-3) to (2-5);

the volume fraction of water in the organic solvent aqueous solution in the step (2) is preferably 5-25%;

the cooling speed in the step (3) is preferably 1-3 ℃/min;

the conditions of the molecular distillation described in step (4) are preferably:

controlling the distillation temperature of 200-;

an apocynum venetum sterol extract is prepared by the above preparation method;

the apocynum venetum sterol extract can be further esterified;

the apocynum venetum sterol extract is applied to the field of preparation of feed additives;

the addition amount of the apocynum venetum sterol extract in the feed is preferably as follows: 50-200 g/ton of poultry feed, 250 g/ton of pig feed and 250 g/ton of aquatic feed;

the apocynum venetum is rich in various sterols such as: beta-sitosterol, stigmasterol, campesterol, sitostanol and the like, the total sterol content can reach more than 370mg/100g, and is higher than the content of common vegetable oil (soybean oil: 307mg/100g and peanut oil: 245mg/100g) in diet, is one of good raw materials for obtaining the phytosterol, the apocynum venetum is used as a raw material, an extracting solution containing the apocynum venetum sterol is obtained by adopting a solvent extraction mode, the extracting solution is not concentrated, and a low-temperature crystallization mode is adopted to separate out the sterol crystals in the extracting solution, so that on one hand, the operation is simpler, on the other hand, the filtered filtrate can be directly recycled, the environment is protected, the safety is higher, and the volatilization of an organic solvent is avoided. And after low-temperature crystallization, performing molecular distillation on the crude extract to further enrich the sterol and remove other impurities.

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

(1) the invention adopts the ambary flower as the source of the phytosterol, the prepared phytosterol does not contain harmful components, and compared with the extraction method of taking deodorized distillate or nuts with high oil content as raw materials, the extraction method is simpler, has low cost and is more suitable for industrial production.

(2) The invention adopts the aqueous solvent for extraction, and reduces the dosage of the organic solvent on one hand. On the other hand, the small amount of water is pure, in the subsequent low-temperature crystallization process, the sterol crystallization is facilitated, the crystallization speed can be improved, the crystallization temperature cannot be too low, and the crystallization cost is further reduced.

(3) The invention adopts a low-temperature crystallization form to concentrate and enrich sterol, thereby greatly reducing the possibility of solvent volatilization and leading the solvent to be recycled in a real sense.

(4) The invention adopts molecular distillation technology to further purify sterol, has the characteristics of simple and rapid operation, excellent product quality and the like, and avoids the loss of thermosensitive components.

Detailed Description

The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.