阅读说明：本技术 山茶粕中的茶皂素提取工艺及其在氨基酸洁面皂中的应用 (Process for extracting tea saponin from camellia sinensis dregs and application of tea saponin in amino acid facial soap ) 是由 郭鹏 崔山虎 曾宪群 赵李红 郭洪燃 赵蜜甜 张钰 于 2020-05-29 设计创作，主要内容包括：本发明公开了一种山茶粕中的茶皂素提取工艺及其在氨基酸洁面皂中的应用,属于茶皂素提取技术领域,包括以下步骤：S1、山茶籽的预处理：将山茶籽洗净、粉碎；S2、脱脂：称取已粉碎的干燥的山茶籽,加入有机溶剂进行脱脂处理,得山茶粕；S3、提取茶皂素：将干燥的山茶粕粉碎,加入150～300ml复合提取溶剂,提取1～3h后,过滤得到深红色提取液；所述复合提取溶剂由碳酸二甲酯：乙醇水溶液按照体积比1：1～3的比例调配。本发明通过利用不同物质的极性差异在碳酸二甲酯和乙醇水溶液的相间进行分配,使杂质等成分与茶皂素分离开,通过收集乙醇水溶液,即可降低茶皂素的杂质含量,达到提高产品品质、提高产品得率和纯度、降低成本的效果。(The invention discloses a process for extracting tea saponin from camellia meal and application of the tea saponin in amino acid facial soap, belonging to the technical field of extraction of tea saponin, and comprising the following steps: s1, pretreatment of camellia seeds: cleaning and pulverizing camellia seeds; s2, degreasing: weighing pulverized and dried camellia seeds, and adding an organic solvent for degreasing treatment to obtain camellia meal; s3, extracting tea saponin: crushing dried camellia oleifera abel dregs, adding 150-300 ml of composite extraction solvent, extracting for 1-3 h, and filtering to obtain a dark red extracting solution; the composite extraction solvent is prepared from dimethyl carbonate: ethanol aqueous solution according to the volume ratio of 1: 1-3 in proportion. The invention separates the components such as impurities from the tea saponin by distributing the polarity difference of different substances between the dimethyl carbonate and the ethanol aqueous solution, and can reduce the impurity content of the tea saponin by collecting the ethanol aqueous solution, thereby achieving the effects of improving the product quality, improving the product yield and purity and reducing the cost.)

1. The process for extracting the tea saponin from the camellia sinensis dregs is characterized by comprising the following steps of:

s1, pretreatment of camellia seeds: cleaning and pulverizing camellia seeds;

s2, degreasing: weighing pulverized and dried camellia seeds, and adding an organic solvent for degreasing treatment to obtain camellia meal;

s3, extracting tea saponin: crushing dried camellia oleifera abel dregs, adding 150-300 ml of composite extraction solvent, extracting for 1-3 h, and filtering to obtain a dark red extracting solution;

the composite extraction solvent is prepared from dimethyl carbonate: ethanol aqueous solution according to the volume ratio of 1: 1-3 in proportion.

2. The extraction process of tea saponin from the camellia sinensis dregs as claimed in claim 1, wherein the composite extraction solvent is prepared from dimethyl carbonate: ethanol aqueous solution according to the volume ratio of 1: 1.4-2.6.

3. The process for extracting tea saponin from camellia meal as claimed in claim 2, wherein the composite extraction solvent is prepared from dimethyl carbonate: ethanol aqueous solution according to the volume ratio of 1: 1.8 in proportion.

4. The extraction process of tea saponin from the camellia sinensis dregs as claimed in claim 1, wherein the concentration of the ethanol aqueous solution is 30-50%.

5. The extraction process of tea saponin from the camellia sinensis dregs as claimed in claim 4, wherein the concentration of the ethanol aqueous solution is 40%.

6. The extraction process of tea saponin from the camellia sinensis dregs as claimed in claim 1, wherein in step S2, the organic solvent is n-hexane.

7. The extraction process of tea saponin from the camellia sinensis dregs as claimed in claim 1, wherein the extraction temperature is 60 ℃ in step S3.

8. The extraction process of tea saponin from the camellia sinensis dregs as claimed in claim 1, wherein in step S3, the filtration is performed by suction filtration.

9. The application of the tea saponin extracted by the tea saponin extraction process in the camellia meal of any one of claims 1-8 in amino acid facial soap.

10. The application of the tea saponin in the amino acid facial soap as claimed in claim 9, wherein the amino acid facial soap comprises the following raw materials in parts by weight: 10-50 parts of tea saponin, 80 parts of cocoyl glutamic acid, 5 parts of triethanolamine, 1 part of glycerol, 3 parts of ethanol and 40 parts of water.

Technical Field

The invention relates to the technical field of tea saponin extraction, in particular to a tea saponin extraction process in camellia sinensis dregs and application of the tea saponin extraction process in amino acid facial soap.

Background

The tea saponin is mainly derived from hydroxyl of Theaceae plant, and is combined with organic acid in various tissue parts of camellia seeds, and is a kind of natural glycoside. It is glycosidically bonded to the carbonyl group of the ligand, wherein the sugar moiety comprises glucuronic acid, arabinose, xylose. The tea saponin is one of natural nonionic surfactants, has excellent performance due to the molecular structure of the tea saponin which has hydrophilic saccharide and hydrophobic groups, is widely applied in the fields of daily chemicals, food, environmental protection and the like, is easy to biodegrade, and cannot pollute the environment.

Due to the wide application, more and more science and technology workers begin to explore the extraction process of tea saponin. At present, the technology for extracting the tea saponin in the camellia sinensis dregs by an alcohol-water solution method is mature. For example, the literature (wang liang, honor, response surface method ultrasonic wave auxiliary extraction tea saponin process optimization [ J ]. water college bulletin, 2014,036(002):23-28.) discloses a response surface method ultrasonic wave auxiliary extraction tea saponin process optimization, which establishes a tea saponin extraction process with 75% ethanol as an extractant, a feed liquid pH value of 8.0, an extraction temperature of 40 ℃, an extraction time of 4h, a liquid-solid ratio of 8:1 and an ultrasonic wave power of 80W, and at the moment, the actual extraction rate of tea saponin is 8.041%. In addition, a research on the extraction and separation process of tea saponin in tea seed meal is disclosed in a document (research on the extraction and separation process of tea saponin in Tang Pengcheng, Wang Wenyuan, Zhu Longjun. tea seed meal [ J ]. chemical engineering management, 2017,000(002):185-186.) and a research on the extraction and separation process of tea saponin in tea seed meal is carried out by a single factor from influencing factors such as pH, temperature, feed-liquid ratio, ethanol concentration and the like, and the yield of tea saponin does not exceed 14% under the optimal condition. However, the ethanol concentration in the prior art usually needs to be higher to achieve better extraction rate and purity, and the high-concentration ethanol can reduce the solubility of the tea saponin, so that the yield of the tea saponin is reduced because the tea saponin is insoluble in pure ethanol; secondly, the alcohol solution is adopted, and due to the strong polarity of the extracting agent, a large amount of impurity components (starch, polysaccharide, vegetable protein and the like) are slightly leached into the extracting agent, so that the tea saponin has the advantages of large viscosity, dark color, low content and low purity.

Disclosure of Invention

The invention aims at the existing technical problems, develops a tea saponin extraction process in camellia meal, and provides application of tea saponin extracted by the tea saponin extraction process in camellia meal in amino acid facial soap; the invention separates the components such as impurities from the tea saponin by distributing the polarity difference of different substances between the dimethyl carbonate and the ethanol aqueous solution, and can reduce the impurity content of the tea saponin by collecting the ethanol aqueous solution, thereby achieving the effects of improving the product quality, improving the product yield and purity and reducing the cost.

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

the process for extracting the tea saponin from the camellia sinensis dregs comprises the following steps:

s1, pretreatment of camellia seeds: cleaning and pulverizing camellia seeds;

s2, degreasing: weighing pulverized and dried camellia seeds, and adding an organic solvent for degreasing treatment to obtain camellia meal;

s3, extracting tea saponin: crushing dried camellia oleifera abel dregs, adding 150-300 ml of composite extraction solvent, extracting for 1-3 h, and filtering to obtain a dark red extracting solution;

the composite extraction solvent is prepared from dimethyl carbonate: ethanol aqueous solution according to the volume ratio of 1: 1-3 in proportion.

Adopt above-mentioned technical scheme: the tea saponin contains a large amount of polar groups such as hydroxyl, carboxyl, carbonyl and the like, is a strong-polarity substance and is very easy to dissolve in an aqueous solution, but impurities such as soluble polysaccharide and the like are easy to leach out, so that the concentration of ethanol in the tea saponin is controlled through a large amount of experiments, and meanwhile, the low-polarity dimethyl carbonate is added to reduce the polarity of an extraction solvent, so that the polarity of the extraction solvent is maintained to be easy to leach out the tea saponin, and the soluble polysaccharide is not easy to leach out; in addition, substances with high hydrocarbon content, such as vegetable protein, fat and other weakly polar or nonpolar fat-soluble substances, are insoluble in ethanol aqueous solution and tend to be dissolved in dimethyl carbonate; therefore, by utilizing the principle of similarity and intermiscibility, different substances are distributed at different phases through polarity difference, so that components such as impurities and the like are separated from the tea saponin, namely, the ethanol water solution is collected, so that the impurity content of the tea saponin can be reduced, and the effects of improving the product quality, improving the product yield and purity and reducing the cost are achieved.

Further, the composite extraction solvent is prepared from dimethyl carbonate: ethanol aqueous solution according to the volume ratio of 1: 1.4-2.6.

Further, the composite extraction solvent is prepared from dimethyl carbonate: ethanol aqueous solution according to the volume ratio of 1: 1.8 in proportion. Dimethyl carbonate: the proportion of the ethanol aqueous solution can obviously influence the polarity change of the composite extraction solvent, and further influence the distribution coefficient of different substances among phases. When the ratio of dimethyl carbonate: when the proportion of the ethanol aqueous solution is low, that is, the content of dimethyl carbonate is low, the content of the ethanol aqueous solution is high, the content of other impurities such as leached polysaccharide, vegetable protein and the like is increased in the proportion of the ethanol aqueous solution, and when the proportion of dimethyl carbonate: when the proportion ratio of the ethanol water solution is high, namely the content of the dimethyl carbonate is high and the content of the ethanol water solution is low, the leaching rate of the tea saponin is low. Thus, the present invention prefers dimethyl carbonate through a number of experiments: the proportion of 50% ethanol aqueous solution is 1: 1.4 to 2.6, most preferably 1: 1.8.

further, the concentration of the ethanol water solution is 30-50%.

Further, the concentration of the ethanol water solution is 40%. The change of the concentration of the ethanol water solution influences the polarity change of the ethanol water solution, and further influences the alternate distribution of the tea saponin in the ethanol water solution. When the concentration of the ethanol is low, water-soluble substances such as polysaccharide and the like are easy to leach, and when the concentration of the ethanol is high, the leaching rate of the tea saponin is low, and only by matching the ethanol with proper concentration with the dimethyl carbonate to properly reduce the polarity of an extraction solvent, the leaching of impurities can be greatly reduced, and meanwhile, the higher yield and the higher purity of the tea saponin are maintained.

Further, in step S2, the organic solvent is n-hexane.

Further, in step S3, the extraction temperature is 60 ℃.

Further, in step S3, the filtering is performed by suction filtration.

The invention also provides application of the tea saponin extracted by the tea saponin extraction process in the camellia sinensis dregs in amino acid facial soap.

The amino acid facial soap comprises the following raw materials in parts by weight: 10-50 parts of tea saponin, 80 parts of cocoyl glutamic acid, 5 parts of triethanolamine, 1 part of glycerol, 3 parts of ethanol and 40 parts of water.

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

1. the invention separates the components such as impurities from the tea saponin by utilizing the similarity and intermiscibility principle and utilizing the polarity difference of different substances to distribute among dimethyl carbonate and ethanol water solution, and can reduce the impurity content of the tea saponin by collecting the ethanol water solution, thereby achieving the effects of improving the product quality, improving the product yield and purity and reducing the cost.

2. According to the invention, through a large number of experiments, proper dimethyl carbonate and ethanol aqueous solution and proportion and proper ethanol concentration are selected, so that the yield of the tea saponin is greatly improved, and under the optimal condition, the extraction rate of the tea saponin is higher than 17%, the purity is higher than 89%, and the product quality is good.

Detailed Description

The technical solution of the present invention will be clearly and completely described below with reference to specific embodiments. It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without any inventive step, are within the scope of the present invention.