CN111592578B - Process for extracting tea saponin from camellia sinensis dregs and application of tea saponin in amino acid facial soap - Google Patents
Process for extracting tea saponin from camellia sinensis dregs and application of tea saponin in amino acid facial soap Download PDFInfo
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- 239000001397 quillaja saponaria molina bark Substances 0.000 title claims abstract description 117
- 229930182490 saponin Natural products 0.000 title claims abstract description 117
- 150000007949 saponins Chemical class 0.000 title claims abstract description 115
- 238000000034 method Methods 0.000 title claims abstract description 14
- 230000008569 process Effects 0.000 title claims abstract description 8
- 244000269722 Thea sinensis Species 0.000 title claims description 23
- 235000006468 Thea sinensis Nutrition 0.000 title claims description 15
- 239000000344 soap Substances 0.000 title abstract description 28
- 230000001815 facial effect Effects 0.000 title abstract description 24
- 150000001413 amino acids Chemical class 0.000 title abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 165
- 238000000605 extraction Methods 0.000 claims abstract description 73
- 239000002904 solvent Substances 0.000 claims abstract description 41
- 239000007864 aqueous solution Substances 0.000 claims abstract description 36
- 240000001548 Camellia japonica Species 0.000 claims abstract description 32
- 235000018597 common camellia Nutrition 0.000 claims abstract description 32
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000002131 composite material Substances 0.000 claims abstract description 30
- 239000000243 solution Substances 0.000 claims abstract description 23
- 235000012054 meals Nutrition 0.000 claims abstract description 13
- 238000005238 degreasing Methods 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 238000005303 weighing Methods 0.000 claims abstract description 5
- 238000004140 cleaning Methods 0.000 claims abstract description 4
- 238000010298 pulverizing process Methods 0.000 claims abstract description 3
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 14
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 10
- 238000000967 suction filtration Methods 0.000 claims description 5
- 241001122767 Theaceae Species 0.000 abstract description 114
- 239000012535 impurity Substances 0.000 abstract description 15
- 239000000126 substance Substances 0.000 abstract description 14
- 230000000694 effects Effects 0.000 abstract description 8
- 239000003960 organic solvent Substances 0.000 abstract description 5
- 241000526900 Camellia oleifera Species 0.000 abstract description 2
- 235000001014 amino acid Nutrition 0.000 description 19
- 230000002829 reductive effect Effects 0.000 description 12
- 238000002386 leaching Methods 0.000 description 10
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 9
- 238000002474 experimental method Methods 0.000 description 7
- 150000004676 glycans Chemical class 0.000 description 7
- 238000005457 optimization Methods 0.000 description 7
- 229920001282 polysaccharide Polymers 0.000 description 7
- 239000005017 polysaccharide Substances 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 4
- 108010082495 Dietary Plant Proteins Proteins 0.000 description 4
- 230000003247 decreasing effect Effects 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- WHUUTDBJXJRKMK-UHFFFAOYSA-N Glutamic acid Natural products OC(=O)C(N)CCC(O)=O WHUUTDBJXJRKMK-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 3
- 230000003385 bacteriostatic effect Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 235000013922 glutamic acid Nutrition 0.000 description 3
- 239000004220 glutamic acid Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- SRBFZHDQGSBBOR-IOVATXLUSA-N D-xylopyranose Chemical compound O[C@@H]1COC(O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-IOVATXLUSA-N 0.000 description 2
- PYMYPHUHKUWMLA-UHFFFAOYSA-N arabinose Natural products OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 description 2
- SRBFZHDQGSBBOR-UHFFFAOYSA-N beta-D-Pyranose-Lyxose Natural products OC1COC(O)C(O)C1O SRBFZHDQGSBBOR-UHFFFAOYSA-N 0.000 description 2
- 239000010495 camellia oil Substances 0.000 description 2
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 235000018102 proteins Nutrition 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- -1 saponin amino acid Chemical class 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 241000222122 Candida albicans Species 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 240000001008 Dimocarpus longan Species 0.000 description 1
- 241000588724 Escherichia coli Species 0.000 description 1
- 235000000235 Euphoria longan Nutrition 0.000 description 1
- IAJILQKETJEXLJ-UHFFFAOYSA-N Galacturonsaeure Natural products O=CC(O)C(O)C(O)C(O)C(O)=O IAJILQKETJEXLJ-UHFFFAOYSA-N 0.000 description 1
- WHUUTDBJXJRKMK-VKHMYHEASA-N L-glutamic acid Chemical compound OC(=O)[C@@H](N)CCC(O)=O WHUUTDBJXJRKMK-VKHMYHEASA-N 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- BWPGKXYWPBQBPV-MWQJAWBESA-N Theasaponin Chemical compound O([C@H]1[C@H](O)[C@H](O[C@H]([C@@H]1O[C@H]1[C@@H]([C@@H](O)[C@@H](O)CO1)O[C@H]1[C@@H]([C@@H](O)[C@H](O)CO1)O)O[C@H]1CC[C@]2(C)[C@H]3CC=C4[C@@]([C@@]3(CC[C@H]2[C@@]1(CO)C)C)(C)C[C@@H](O)[C@@]1(CO)[C@@H](OC(C)=O)[C@@H](C(C[C@H]14)(C)C)OC(=O)C(\C)=C/C)C(O)=O)[C@@H]1O[C@H](CO)[C@H](O)[C@H](O)[C@H]1O BWPGKXYWPBQBPV-MWQJAWBESA-N 0.000 description 1
- BWPGKXYWPBQBPV-ZOADXXHESA-N Theasaponin Natural products O=C(O[C@@H]1[C@@H](OC(=O)C)[C@]2(CO)[C@@H](O)C[C@@]3(C)[C@@]4(C)[C@@H]([C@]5(C)[C@H]([C@@](CO)(C)[C@@H](O[C@@H]6[C@@H](O[C@@H]7[C@H](O[C@@H]8[C@@H](O)[C@H](O)[C@H](O)CO8)[C@H](O)[C@@H](O)CO7)[C@@H](O[C@H]7[C@H](O)[C@@H](O)[C@@H](O)[C@H](CO)O7)[C@H](O)[C@@H](C(=O)O)O6)CC5)CC4)CC=C3[C@@H]2CC1(C)C)/C(=C/C)/C BWPGKXYWPBQBPV-ZOADXXHESA-N 0.000 description 1
- IAJILQKETJEXLJ-QTBDOELSSA-N aldehydo-D-glucuronic acid Chemical compound O=C[C@H](O)[C@@H](O)[C@H](O)[C@H](O)C(O)=O IAJILQKETJEXLJ-QTBDOELSSA-N 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- PYMYPHUHKUWMLA-WDCZJNDASA-N arabinose Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)C=O PYMYPHUHKUWMLA-WDCZJNDASA-N 0.000 description 1
- 230000017531 blood circulation Effects 0.000 description 1
- 229940095731 candida albicans Drugs 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 238000004925 denaturation Methods 0.000 description 1
- 230000036425 denaturation Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 229940097043 glucuronic acid Drugs 0.000 description 1
- 229930182470 glycoside Natural products 0.000 description 1
- 150000002338 glycosides Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 125000001165 hydrophobic group Chemical group 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012543 microbiological analysis Methods 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000005063 solubilization Methods 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07J—STEROIDS
- C07J63/00—Steroids in which the cyclopenta(a)hydrophenanthrene skeleton has been modified by expansion of only one ring by one or two atoms
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/20—Carbocyclic rings
- C07H15/24—Condensed ring systems having three or more rings
- C07H15/256—Polyterpene radicals
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
- C11D1/83—Mixtures of non-ionic with anionic compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/20—Organic compounds containing oxygen
- C11D3/2003—Alcohols; Phenols
- C11D3/2065—Polyhydric alcohols
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/26—Organic compounds containing nitrogen
- C11D3/30—Amines; Substituted amines ; Quaternized amines
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/04—Carboxylic acids or salts thereof
- C11D1/10—Amino carboxylic acids; Imino carboxylic acids; Fatty acid condensates thereof
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
- C11D1/662—Carbohydrates or derivatives
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- General Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Emergency Medicine (AREA)
- Steroid Compounds (AREA)
- Medicines Containing Plant Substances (AREA)
- Cosmetics (AREA)
Abstract
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.
Description
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.
Example 1 extraction of tea saponin from camellia sinensis seed meal
The main reagents and raw materials in this example: camellia seeds; n-hexane (AR grade); ethanol (AR grade); methanol (AR grade); water (AR grade); dimethyl carbonate (AR grade).
The tea saponin extraction process in the camellia sinensis dregs comprises the following steps:
s1, pretreatment of camellia seeds: cleaning camellia seeds, putting the camellia seeds into a container, controlling time, and crushing the camellia seeds into fine particles;
s2, degreasing: weighing 50g of crushed dried camellia seeds, placing the crushed dried camellia seeds in a 500ml beaker, adding 150ml of normal hexane, stirring for 2 hours to obtain tea oil, collecting and utilizing the tea oil, and drying the remaining components to obtain camellia meal;
s3, extracting tea saponin: crushing dried camellia meal, putting the crushed camellia meal into a conical flask, adding 150-300 ml of a composite extraction solvent, extracting at 60 ℃ for 1-3 h, and performing suction filtration by using a suction filtration device 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.
According to experiments, the dissolving amount of the tea saponin in the ethanol water solution can be increased along with the increase of the material-liquid ratio, and meanwhile, the concentration of the tea saponin in the solution is reduced, the mass transfer power is increased, and the leaching of substances is facilitated; but when the ratio of the camellia seeds to the composite extraction solvent is between 3 and 6, along with the increase of the ratio of the camellia seeds to the composite extraction solvent, the increase of the yield of the tea saponin is not obvious, so that the application needs smaller ratio of the camellia seeds to the composite extraction solvent based on the cost consideration, the suction filtration and other processes, and the comprehensive consideration adopts 1: 4 ratio of material to liquid. Meanwhile, the leaching time has certain influence on the yield of the tea saponin, and multiple experiments show that after the seed cake is soaked for 3 hours, the tea saponin basically reaches balance in a liquid phase, so that the seed cake is soaked for 3 hours in actual production. That is, in the following examples, unless otherwise specified, the ratio of camellia seeds to the composite extraction solvent is 1: 4, in step S2, weighing 50g camellia seeds, and in step S4, extracting for 3h with 200ml of composite extraction solvent.
Example 2 optimization of the compounding of extraction solvent
a) Optimization of composite extraction solvent composition
The kind of the extraction solvent has certain influence on the content and yield of the tea saponin. Selecting different degreasing organic solvents (n-hexane and dimethyl carbonate) and extraction solvents (ethyl acetate, ethanol, chloroform and 50% ethanol water) and dimethyl carbonate according to the proportion of 1:1 compounding, extracting the tea saponin by the steps of the example 1, and determining the content and the purity of the tea saponin by adopting a vanillin-concentrated sulfuric acid colorimetric method (wandering clouds, Zhengshan yoga, Chenyan, and the like, research on the extraction process of the tea saponin in longan tea dregs [ J ] application chemical industry 2015,000(009): 1635-. And (3) investigating the influence of different composite extraction solvents on the yield and the purity of the tea saponin.
TABLE 1 quality of tea saponin obtained with different extraction solvents
As can be seen from table 1, if the camellia sinensis dregs are extracted by ethyl acetate, the content, yield and purity of the final tea saponin are lower. If chloroform is used as the leaching liquor, although the quality of the obtained tea saponin is obviously improved, the adoption of the process has high requirement on the precision of equipment and needs a large amount of organic solvent, so the adoption of the alcohol-water solution method is more ideal; and carrying out degreasing treatment by adopting normal hexane, and then carrying out degreasing treatment by using 50% ethanol water: the content and purity of the obtained tea saponin are higher by the extraction of the composite extraction solvent of the dimethyl carbonate, so that the composite extraction solvent is optimized subsequently to further improve the content and purity of the tea saponin.
b) Optimization of composite extraction solvent ratio
The composite extraction solvent is prepared from dimethyl carbonate: the proportion of 50% ethanol aqueous solution is respectively 1:1. 1:1.4, 1:1.8, 1: 2.2, 1:2.6, 1: 3, the steps of example 1 are used to extract tea saponin, and the influence of the mixture ratio of the compound extraction solvent on the yield and purity of tea saponin is examined.
TABLE 2 quality of tea saponin obtained by different ratios of composite extraction solvent
As can be seen from table 2, the yield and purity of tea saponin can be increased by properly increasing the amount of 50% ethanol aqueous solution, because tea saponin is dissolved in ethanol aqueous solution, but as the amount of ethanol aqueous solution is further increased, that is, the content of dimethyl carbonate is decreased, the yield is slightly increased, but the purity is decreased, most of tea saponin is leached, and further increasing the proportion of ethanol aqueous solution causes the content of other impurities such as leached polysaccharide, vegetable protein and the like to be increased in the ethanol aqueous solution, thereby causing the purity to be decreased, and when the amount of dimethyl carbonate is increased: the proportion of 50% ethanol aqueous solution is 1:2.6, the impurities are leached in a large amount, the concentration of the composite extraction solvent is obviously increased, the mass transfer power is reduced, the leaching speed is reduced, and the yield of the tea saponin is further influenced. Therefore, dimethyl carbonate was chosen: the proportion of 50% ethanol aqueous solution is 1: 1.4-2.6 is a better ratio, 1:1.8 is the best mixture ratio.
c) Optimization of concentration of ethanol aqueous solution in composite extraction solvent
The composite extraction solvent is prepared from dimethyl carbonate: the proportion of ethanol aqueous solution is respectively 1:1.8, 20%, 30%, 40%, 50% and 60% of ethanol aqueous solution respectively, extracting the tea saponin by the steps of example 1, and investigating the influence of the ethanol aqueous solution of the compound extraction solvent on the yield and purity of the tea saponin.
TABLE 3 quality of tea saponin obtained from different ethanol aqueous solutions in the composite extraction solvent
As can be seen from Table 3, the effect of extracting tea saponin by combining an ethanol aqueous solution with a certain concentration and dimethyl carbonate is better than that of extracting a low-concentration or high-concentration ethanol aqueous solution, that is, the extraction rate of tea saponin is increased and then decreased along with the increase of the ethanol concentration, mainly because water-soluble substances such as polysaccharide and the like are easy to leach when the ethanol concentration is lower in the leaching process, and the combination of ethanol with dimethyl carbonate with a certain concentration can properly reduce the polarity of an extraction solvent, greatly reduce the leaching of impurities and improve the yield of tea saponin, but the yield of tea saponin is reduced along with the continuous increase of the ethanol concentration, the purity is obviously reduced along with the decrease of the ethanol concentration when the ethanol concentration exceeds 50 percent, because the polarity is obviously reduced along with the increase of the ethanol concentration, the denaturation and solidification of substances such as protein and the like are accelerated, the leaching reaction is prevented from continuing, and the polarity of the extraction solvent is also obviously reduced, resulting in micro-solubilization of soluble proteins and the tea saponin is insoluble in anhydrous ethanol.
Example 3 optimization of extraction temperature
The composite extraction solvent is prepared from dimethyl carbonate: the proportion of 40% ethanol aqueous solution is respectively 1:1.8, the procedure of example 1 was followed to extract tea saponin at different temperatures and examine the effect of temperature on the yield and purity of tea saponin.
TABLE 4 quality of tea saponin obtained under different temperature conditions
Through a series of experiments, the yield of the tea saponin can be increased and the color can be deepened along with the increase of the temperature in a certain temperature range, but the yield of the tea saponin can be reduced along with the continuous increase of the temperature, so that the temperature of 60 ℃ is the optimum extraction temperature, and the quality of the tea saponin is high under the temperature condition.
Example 4 application of tea saponin to amino acid facial soap
Pouring the extracted tea saponin into a beaker, putting a certain amount of cocoyl glutamic acid and glycerol into the beaker, heating to 70 ℃, fully stirring by using a magnetic stirrer until no solid exists in the solution, standing, adding a proper amount of triethanolamine into the beaker, quickly pouring into a mould after uniformly stirring, adding alcohol into the mould to eliminate foam, standing for one month, observing the shape and the like of the 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.
For different addition amounts of tea saponin facial soap, the antibacterial rates (50%, 5min) of Escherichia coli, Staphylococcus aureus and Candida albicans were measured in the center of microbiological analysis and detection. Meanwhile, the influence of the addition amount of the tea saponin extracting solution on the color of the tea saponin facial soap is analyzed, and the experimental results are respectively shown in tables 5-6.
TABLE 5 bacteriostatic ability of different addition amounts of theasaponin facial soap
TABLE 6 influence of different addition amounts of tea saponin on the color of tea saponin facial soap
As can be seen from tables 5-6, the tea saponin extracted by the method is high in purity, and when the tea saponin is added into the amino acid facial soap, the dirt-removing capacity and the bacteriostatic capacity of the amino acid facial soap can be improved, and the tea saponin amino acid facial soap can accelerate the blood circulation of skin and has the bacteriostatic and protective effects on local infection. And secondly, the amino acid facial soap has good appearance and high stability, and does not have the phenomena of precipitation, delamination and the like after being placed for one month at room temperature.
Further experiments show that when the amino acid facial soap is prepared into a solid product, 5 g, 10 g, 15 g, 20 g, 25 g and 30 g of tea saponin are respectively added into the amino acid facial soap, the detergency of the amino acid facial soap is measured, and the detergency of the amino acid facial soap is increased with the increase of the addition amount of the tea saponin, but the detergency of the amino acid facial soap is reduced instead due to the following reasons: the excessive addition of the tea saponin has an inhibiting effect on the activity of the tea saponin, and the detergency of the tea saponin facial soap is influenced under the interaction of several surfactants; the cleansing soap added with 20 g of tea saponin has the strongest dirt-removing power, and the same experimental results are obtained by comparing the tea saponin amino acid cleansing soaps prepared by different formulas, so that the cleansing soap obtained by preferably adding 20 g of tea saponin into each amino acid cleansing soap has the advantages of strong dirt-removing power, high activity content and good stability.
Claims (5)
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 n-hexane for degreasing treatment to obtain camellia meal;
s3, extracting tea saponin: crushing dried camellia sinensis dregs, adding a composite extraction solvent, extracting for 3 hours, and filtering to obtain a dark red extracting solution; the ratio of the volume usage amount of the composite extraction solvent to the weight of the camellia seeds is 4 mL/g;
the composite extraction solvent is prepared from dimethyl carbonate: the ethanol aqueous solution is prepared according to the volume ratio of 1: 1.4-1: 2.6; the concentration of the ethanol water solution is 30-50%.
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: the ethanol aqueous solution is prepared according to the volume ratio of 1: 1.8.
3. 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 40%.
4. 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.
5. 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.
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