CN116789715A - Extraction process of water-soluble saponin - Google Patents
Extraction process of water-soluble saponin Download PDFInfo
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- CN116789715A CN116789715A CN202310746277.8A CN202310746277A CN116789715A CN 116789715 A CN116789715 A CN 116789715A CN 202310746277 A CN202310746277 A CN 202310746277A CN 116789715 A CN116789715 A CN 116789715A
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- saponin
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- ethyl alcohol
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- 239000001397 quillaja saponaria molina bark Substances 0.000 title claims abstract description 154
- 229930182490 saponin Natural products 0.000 title claims abstract description 154
- 150000007949 saponins Chemical class 0.000 title claims abstract description 154
- 238000000605 extraction Methods 0.000 title claims abstract description 31
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 120
- 239000002253 acid Substances 0.000 claims abstract description 77
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 62
- 239000002904 solvent Substances 0.000 claims abstract description 61
- 239000003208 petroleum Substances 0.000 claims abstract description 60
- 239000007787 solid Substances 0.000 claims abstract description 40
- 239000000463 material Substances 0.000 claims abstract description 20
- 239000007788 liquid Substances 0.000 claims abstract description 19
- 238000000926 separation method Methods 0.000 claims abstract description 18
- 238000004064 recycling Methods 0.000 claims abstract description 11
- 235000019441 ethanol Nutrition 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims description 28
- 241000196324 Embryophyta Species 0.000 claims description 16
- 238000010828 elution Methods 0.000 claims description 14
- 230000003301 hydrolyzing effect Effects 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- VFLDPWHFBUODDF-FCXRPNKRSA-N curcumin Chemical group C1=C(O)C(OC)=CC(\C=C\C(=O)CC(=O)\C=C\C=2C=C(OC)C(O)=CC=2)=C1 VFLDPWHFBUODDF-FCXRPNKRSA-N 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 235000014375 Curcuma Nutrition 0.000 claims 1
- 244000164439 Curcuma angustifolia Species 0.000 claims 1
- 210000000582 semen Anatomy 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 15
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 5
- 230000007062 hydrolysis Effects 0.000 abstract description 4
- 238000010364 biochemical engineering Methods 0.000 abstract description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 24
- DWCSNWXARWMZTG-UHFFFAOYSA-N Trigonegenin A Natural products CC1C(C2(CCC3C4(C)CCC(O)C=C4CCC3C2C2)C)C2OC11CCC(C)CO1 DWCSNWXARWMZTG-UHFFFAOYSA-N 0.000 description 9
- WQLVFSAGQJTQCK-VKROHFNGSA-N diosgenin Chemical compound O([C@@H]1[C@@H]([C@]2(CC[C@@H]3[C@@]4(C)CC[C@H](O)CC4=CC[C@H]3[C@@H]2C1)C)[C@@H]1C)[C@]11CC[C@@H](C)CO1 WQLVFSAGQJTQCK-VKROHFNGSA-N 0.000 description 9
- WQLVFSAGQJTQCK-UHFFFAOYSA-N diosgenin Natural products CC1C(C2(CCC3C4(C)CCC(O)CC4=CCC3C2C2)C)C2OC11CCC(C)CO1 WQLVFSAGQJTQCK-UHFFFAOYSA-N 0.000 description 9
- 239000002351 wastewater Substances 0.000 description 9
- 244000062245 Hedychium flavescens Species 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 230000003472 neutralizing effect Effects 0.000 description 6
- 239000003814 drug Substances 0.000 description 5
- 239000002699 waste material Substances 0.000 description 5
- 244000163122 Curcuma domestica Species 0.000 description 4
- 235000003392 Curcuma domestica Nutrition 0.000 description 4
- 235000003373 curcuma longa Nutrition 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 239000003270 steroid hormone Substances 0.000 description 4
- 235000013976 turmeric Nutrition 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 244000281702 Dioscorea villosa Species 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- 241000361919 Metaphire sieboldi Species 0.000 description 3
- 235000004879 dioscorea Nutrition 0.000 description 3
- 229940079593 drug Drugs 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 240000001980 Cucurbita pepo Species 0.000 description 1
- 235000009852 Cucurbita pepo Nutrition 0.000 description 1
- 235000005903 Dioscorea Nutrition 0.000 description 1
- 235000017008 Dioscorea nipponica Nutrition 0.000 description 1
- 241000908494 Dioscorea nipponica Species 0.000 description 1
- 235000000504 Dioscorea villosa Nutrition 0.000 description 1
- QOLRLLFJMZLYQJ-LOBDNJQFSA-N Hecogenin Chemical compound O([C@@H]1[C@@H]([C@]2(C(=O)C[C@@H]3[C@@]4(C)CC[C@H](O)C[C@@H]4CC[C@H]3[C@@H]2C1)C)[C@@H]1C)[C@]11CC[C@@H](C)CO1 QOLRLLFJMZLYQJ-LOBDNJQFSA-N 0.000 description 1
- OXLGJTRVVNGJRK-UHFFFAOYSA-N Hecogenin Natural products CC1CCC2(CC3CC4C5CCC6CC(O)CCC6(C)C5CC(=O)C4(C)C3C2C)OC1 OXLGJTRVVNGJRK-UHFFFAOYSA-N 0.000 description 1
- UVLDESQWQRMYKD-UHFFFAOYSA-N Neobotogenin Natural products CC1C(C2(C(=O)CC3C4(C)CCC(O)CC4=CCC3C2C2)C)C2OC11CCC(C)CO1 UVLDESQWQRMYKD-UHFFFAOYSA-N 0.000 description 1
- 108010009736 Protein Hydrolysates Proteins 0.000 description 1
- GMBQZIIUCVWOCD-WWASVFFGSA-N Sarsapogenine Chemical compound O([C@@H]1[C@@H]([C@]2(CC[C@@H]3[C@@]4(C)CC[C@H](O)C[C@H]4CC[C@H]3[C@@H]2C1)C)[C@@H]1C)[C@]11CC[C@H](C)CO1 GMBQZIIUCVWOCD-WWASVFFGSA-N 0.000 description 1
- RTMWIZOXNKJHRE-UHFFFAOYSA-N Tigogenin Natural products CC1COC2CC(C)(OC12)C3CCC4C5CCC6CC(O)CCC6(C)C5CCC34C RTMWIZOXNKJHRE-UHFFFAOYSA-N 0.000 description 1
- 244000250129 Trigonella foenum graecum Species 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 125000001483 monosaccharide substituent group Chemical group 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07G—COMPOUNDS OF UNKNOWN CONSTITUTION
- C07G3/00—Glycosides
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Steroid Compounds (AREA)
Abstract
The application belongs to the technical field of biochemical engineering, and particularly relates to an extraction process of water-soluble saponin. The application provides an extraction process of water-soluble saponin, which comprises the following steps: adding acid liquor and petroleum ether solvent into the saponin extract obtained by alcohol extraction for hydrolysis and saponin extraction; separating the materials to obtain solid, petroleum ether solvent and acid liquor dissolved with water-soluble saponin, and directly returning the acid liquor dissolved with water-soluble saponin to the step 1) for repeated use; eluting the solid obtained by separating the materials by using absolute ethyl alcohol; concentrating and crystallizing the absolute ethyl alcohol dissolved with the water-soluble saponin by solid-liquid separation to obtain the water-soluble saponin, condensing and recycling the concentrated and separated absolute ethyl alcohol, and returning the condensed and separated absolute ethyl alcohol to the step 3) for repeated use. The method integrates the sequence of multiple steps, increases the separation of the water-soluble saponin, and further improves the yield of the saponin.
Description
The application relates to a divisional application of a water-soluble saponin extraction process with the application date of 2019, 05 month and 15 days, the application number of CN 201910402468.6.
Technical Field
The application belongs to the technical field of biochemical engineering, and particularly relates to an extraction process of water-soluble saponin.
Background
The saponin is white crystal or powder, has melting point of 195-205 deg.c, is insoluble in water, and is easy to dissolve in benzene, chloroform and other organic solvents, and is the basic material for producing steroid hormone medicine. The plant saponin mainly comprises three main categories, namely diosgenin, tigogenin and hecogenin, wherein the diosgenin is the most ideal basic raw material for producing steroid hormone medicines, and more than two thirds of the world steroid hormone medicines are produced by taking the diosgenin as the basic raw material, so the diosgenin has very important roles in the production of the steroid hormone medicines. The plant resources with higher yam saponin content in the world are not more and are mainly distributed in China and Mexico, so China and Mexico are large countries for producing yam saponin. In mexico, the plants with higher diosgenin content are mainly dioscorea spica. In China, plants containing diosgenin have seventeen kinds, but have higher content and industrial development value mainly including yellow ginger, earthworm and common fenugreek. The content of the diosgenin is only half of that of yellow ginger (about 2.5% of that of dried yellow ginger and 1.2% of that of the diosgenin), the growth cycle is higher than that of yellow Jiang Chang (2 years of yellow ginger and 4-5 years of that of the diosgenin), and the content of the cucurbita pepo seed saponin is lower (0.8% -1.2%), so that the yellow ginger becomes the most main medicine source plant for producing saponin in China.
The traditional process steps for extracting saponin from yellow ginger or Chuanlong earthworm are as follows: pulverizing rhizoma Dioscoreae Zingiberensis or Dioscorea nipponica Makino, extracting with solvent to obtain saponin, hydrolyzing with acid, washing with water, oven drying to obtain hydrolysate, adding solvent, and separating solid from liquid to obtain saponin. The pollution existing in the traditional process is mainly water pollution, and the traditional process is based on the production statistics of manually planted turmeric, 130-180 tons of fresh turmeric are needed for each 1 ton of saponin production, 15-20 tons of industrial hydrochloric acid (35 wt%) and 500 tons of wastewater are discharged averagely. In addition, about 10 tons of turmeric waste residue is discharged per 1 ton of saponin production. The saponin production wastewater belongs to acid-containing high-concentration organic wastewater and is characterized in that: poor biodegradability: BOD:8000mg/L; BOD/COD of about 0.27; high sugar content: the total sugar content of the comprehensive wastewater is about 2%, and most of the comprehensive wastewater is monosaccharide; pollution load: COD: 20000-30000 mg/L (comprehensive waste water wherein the first-pass liquid (approximately 20% of the waste water amount, COD 110000 mg/L)); the acidity is high: PH:1.0 to 2.5; the salt content is high: in wastewater at ph=1.0; cl - :9600mg/L (HCl hydrolysis process) or SO 4 2- ：9300mg/L(H 2 SO 4 Hydrolysis process);these salts remained after neutralization (Cl - ) Or most remain (SO 4 2- ) Ammonia nitrogen pollution exists, and the concentration is about 500 mg/L; there is a pollution of chromaticity, and the concentration is about 3500 times.
In addition, besides the oil-soluble saponin which can be extracted by the traditional process, the plant also contains a large amount of water-soluble saponin which is not extracted, but is adhered to a solid byproduct or is dissolved in waste acid to be discarded, so that the extraction rate of the saponin can not be further improved.
Disclosure of Invention
The application aims to solve the technical problems that: overcomes the defects of the prior art and provides an extraction process of water-soluble saponin with high extraction rate.
In order to achieve the above object, the present application provides the following technical solutions:
an extraction process of water-soluble saponin comprises the following steps:
1) The plant part adopts an alcohol extraction process to obtain a saponin extract, and acid liquor and petroleum ether solvent are simultaneously added into the saponin extract to carry out saponin extraction while hydrolyzing; the mass ratio of the saponin extract to the petroleum ether solvent to the acid solution is 1:1.4:0.6;
2) Separating out solid, petroleum ether solvent and acid solution dissolved with water-soluble saponin by using a three-phase separator after the step 1) is completed, washing the acid solution dissolved with water-soluble saponin by using petroleum ether solvent for 2 times, and returning the acid solution to the step 1) for repeated use so as to continuously improve the concentration of the water-soluble saponin in the acid solution, wherein the volume ratio of the acid solution dissolved with water-soluble saponin to the total amount of the petroleum ether solvent for washing is 10:2;
3) Drying the solid obtained by separating the materials, adding the dried solid into an elution kettle preloaded with absolute ethyl alcohol, and simultaneously starting stirring; the mass ratio of the solid obtained by separating the materials to the absolute ethyl alcohol is 1:5, a step of; repeating for 3 times;
4) Then carrying out solid-liquid separation to obtain absolute ethyl alcohol in which water-soluble saponin is dissolved; and (3) concentrating and crystallizing the absolute ethyl alcohol dissolved with the water-soluble saponin to obtain the water-soluble saponin, condensing and recycling the concentrated and separated absolute ethyl alcohol, and returning the concentrated and separated absolute ethyl alcohol to the step (3) for repeated use.
Preferably, the plant parts in the process are turmeric, earthworm and common in the industry.
The water-soluble saponin in the traditional process is generally attached to a solid byproduct or dissolved in waste acid to be discarded. The inventor of the application realizes the recycling of waste acid in the early application technology, thereby realizing the continuous enrichment of water-soluble saponin. Then petroleum ether and acid liquor are mixed to extract the water-soluble saponin by means of high concentration of the water-soluble saponin. This way, although a part of the water-soluble saponin is extracted, the yield of the saponin is improved. But this approach is less efficient. Because the solubility of the water-soluble saponin in the acid liquor is relatively large, how to conveniently extract and separate the water-soluble saponin dissolved in the acid liquor becomes a new technical bottleneck encountered by the inventor.
Compared with the prior art, the extraction process of the water-soluble saponin has the beneficial effects that: the method integrates the sequence of a plurality of steps after the alcohol extraction step of the traditional process, and the acid separated in the step 2) contains a small amount of water-soluble saponin, but the water-soluble saponin in the process can be returned to the step 1) together with the acid, so that the waste of discharge is avoided, and the extraction rate of the saponin can be effectively improved. The application realizes the production of saponin without wastewater discharge, the used acid and petroleum ether solvent are in a closed circulation use state, and the process has no other loss except trace residues in separated solids, thereby greatly saving water consumption and acid consumption, and the produced solids can be used later, such as feed. The application takes the separated solid as a break, and the concentration of the water-soluble saponin in the acid liquor is continuously improved on the basis of recycling the acid liquor. The method takes the solid raw material in the reaction process as the adsorption material, and because the concentration of the water-soluble saponin in the acid liquor is higher, part of the water-soluble saponin is necessarily adsorbed on the solid material in the hydrolysis reaction process.
Detailed Description
The following description of the embodiments of the present application will clearly and fully describe the technical solutions of the present application, and it is apparent that the described embodiments are only some embodiments of the present application, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
Example 1
1) The plant part adopts an alcohol extraction process to obtain a saponin extract, and acid liquor and petroleum ether solvent are simultaneously added into the saponin extract to carry out saponin extraction while hydrolyzing; the mass ratio of the saponin extract to the petroleum ether solvent to the sulfuric acid (calculated by the amount of pure sulfuric acid) is 1:1.4:0.6;
2) Separating out solid, petroleum ether solvent and acid liquor dissolved with water-soluble saponin by using a three-phase separator after the step 1) is completed, washing the acid liquor dissolved with water-soluble saponin by using petroleum ether solvent for 2 times, and returning the acid liquor to the step 1) for repeated use to continuously improve the concentration of the water-soluble saponin in the acid liquor, wherein the volume ratio of the acid liquor to the total petroleum ether solvent for washing is 10:2;
3) Drying the solid obtained by separating the materials, adding the dried solid into an elution kettle preloaded with absolute ethyl alcohol, and simultaneously starting stirring; the mass ratio of the solid obtained by separating the materials in the elution kettle to the absolute ethyl alcohol is 1:5, a step of; repeating for 3 times;
4) Then carrying out solid-liquid separation to obtain absolute ethyl alcohol in which water-soluble saponin is dissolved; concentrating and crystallizing the absolute ethyl alcohol dissolved with the water-soluble saponin to obtain the water-soluble saponin, condensing and recycling the concentrated and separated absolute ethyl alcohol, and returning the concentrated and separated absolute ethyl alcohol to the step 3) for repeated use; and (3) mixing the petroleum ether solvent with dissolved saponin obtained by liquid separation with petroleum ether solvent with washing acid, neutralizing, concentrating and crystallizing to obtain oil-soluble saponin, condensing and recovering the concentrated and separated petroleum ether solvent, and returning to the step (1) for extracting the saponin or the step (2) for washing acid. The total yield of saponin in this example was 5.6%.
Example 2
1) The plant part adopts an alcohol extraction process to obtain a saponin extract, and acid liquor and petroleum ether solvent are simultaneously added into the saponin extract to carry out saponin extraction while hydrolyzing; the mass ratio of the saponin extract to the petroleum ether solvent to the sulfuric acid (calculated by the amount of pure sulfuric acid) is 1:1.5:0.5;
2) Separating out solid, petroleum ether solvent and acid liquor dissolved with water-soluble saponin by using a three-phase separator after the step 1) is completed, washing the acid liquor dissolved with water-soluble saponin by using petroleum ether solvent for 2 times, and returning the acid liquor to the step 1) for repeated use to continuously improve the concentration of the water-soluble saponin in the acid liquor, wherein the volume ratio of the acid liquor to the total petroleum ether solvent for washing is 10:2.5;
3) Drying the solid obtained by separating the materials, adding the dried solid into an elution kettle preloaded with absolute ethyl alcohol, and simultaneously starting stirring; the mass ratio of the solid obtained by separating the materials in the elution kettle to the absolute ethyl alcohol is 1:4, a step of; repeating for 3 times;
4) Then carrying out solid-liquid separation to obtain absolute ethyl alcohol in which water-soluble saponin is dissolved; concentrating and crystallizing the absolute ethyl alcohol dissolved with the water-soluble saponin to obtain the water-soluble saponin, condensing and recycling the concentrated and separated absolute ethyl alcohol, and returning the concentrated and separated absolute ethyl alcohol to the step 3) for repeated use; and (3) mixing the petroleum ether solvent with dissolved saponin obtained by liquid separation with petroleum ether solvent with washing acid, neutralizing, concentrating and crystallizing to obtain oil-soluble saponin, condensing and recovering the concentrated and separated petroleum ether solvent, and returning to the step (1) for extracting the saponin or the step (2) for washing acid. The total yield of saponin in this example was 5.5%.
Example 3
1) The plant part adopts an alcohol extraction process to obtain a saponin extract, and acid liquor and petroleum ether solvent are simultaneously added into the saponin extract to carry out saponin extraction while hydrolyzing; the mass ratio of the saponin extract to the petroleum ether solvent to the sulfuric acid (calculated by the amount of pure sulfuric acid) is 1:1.4:0.7;
2) After the step 1) is finished, carrying out solid-liquid separation to obtain solid and liquid phase through filter pressing, standing and separating the liquid phase to obtain petroleum ether solvent and acid liquor dissolved with water-soluble saponin, washing the acid liquor dissolved with water-soluble saponin by using petroleum ether solvent for 1-3 times, and returning the acid liquor to the step 1) for repeated use so as to continuously improve the concentration of the water-soluble saponin in the acid liquor, wherein the volume ratio of the acid liquor to the total petroleum ether solvent for washing is 10:1.5;
3) Drying the solid obtained by separating the materials, adding the dried solid into an elution kettle preloaded with absolute ethyl alcohol, and simultaneously starting stirring; the mass ratio of the solid obtained by separating the materials in the elution kettle to the absolute ethyl alcohol is 1:3.5; repeating for 3 times;
4) Then carrying out solid-liquid separation to obtain absolute ethyl alcohol in which water-soluble saponin is dissolved; concentrating and crystallizing the absolute ethyl alcohol dissolved with the water-soluble saponin to obtain the water-soluble saponin, condensing and recycling the concentrated and separated absolute ethyl alcohol, and returning the concentrated and separated absolute ethyl alcohol to the step 3) for repeated use; and (3) mixing the petroleum ether solvent with dissolved saponin obtained by liquid separation with petroleum ether solvent with washing acid, neutralizing, concentrating and crystallizing to obtain oil-soluble saponin, condensing and recovering the concentrated and separated petroleum ether solvent, and returning to the step (1) for extracting the saponin or the step (2) for washing acid. The total yield of saponin in this example was 5.5%.
Example 4
1) The plant part adopts an alcohol extraction process to obtain a saponin extract, and acid liquor and petroleum ether solvent are simultaneously added into the saponin extract to carry out saponin extraction while hydrolyzing; the mass ratio of the saponin extract to the petroleum ether solvent to the sulfuric acid (calculated by the amount of pure sulfuric acid) is 1:1.6:0.4;
2) Separating out solid, petroleum ether solvent and acid liquor dissolved with water-soluble saponin by using a three-phase separator after the step 1) is completed, washing the acid liquor dissolved with water-soluble saponin by using petroleum ether solvent for 3 times, and returning the acid liquor to the step 1) for repeated use to continuously improve the concentration of the water-soluble saponin in the acid liquor, wherein the volume ratio of the acid liquor to the total petroleum ether solvent for washing is 10:3, a step of;
3) Drying the solid obtained by separating the materials, adding the dried solid into an elution kettle preloaded with absolute ethyl alcohol, and simultaneously starting stirring; the mass ratio of the solid obtained by separating the materials in the elution kettle to the absolute ethyl alcohol is 1:6, preparing a base material; repeating for 4 times;
4) Then carrying out solid-liquid separation to obtain absolute ethyl alcohol in which water-soluble saponin is dissolved; concentrating and crystallizing the absolute ethyl alcohol dissolved with the water-soluble saponin to obtain the water-soluble saponin, condensing and recycling the concentrated and separated absolute ethyl alcohol, and returning the concentrated and separated absolute ethyl alcohol to the step 3) for repeated use; and (3) mixing the petroleum ether solvent with dissolved saponin obtained by liquid separation with petroleum ether solvent with washing acid, neutralizing, concentrating and crystallizing to obtain oil-soluble saponin, condensing and recovering the concentrated and separated petroleum ether solvent, and returning to the step (1) for extracting the saponin or the step (2) for washing acid. The total yield of saponin in this example was 5.3%.
Example 5
1) The plant part adopts an alcohol extraction process to obtain a saponin extract, and acid liquor and petroleum ether solvent are simultaneously added into the saponin extract to carry out saponin extraction while hydrolyzing; the mass ratio of the saponin extract to the petroleum ether solvent to the sulfuric acid (calculated by the amount of pure sulfuric acid) is 1:1.3:0.8;
2) After the step 1), carrying out solid-liquid separation to obtain solid and liquid phase through filter pressing, standing and separating the liquid phase to obtain petroleum ether solvent and acid liquor dissolved with water-soluble saponin, washing the acid liquor dissolved with water-soluble saponin with petroleum ether solvent for 1 time, and returning to the step 1) for repeated use to continuously improve the concentration of the water-soluble saponin in the acid liquor, wherein the volume ratio of the acid liquor to the total petroleum ether solvent for washing is 10:1, a step of;
3) Drying the solid obtained by separating the materials, adding the dried solid into an elution kettle preloaded with absolute ethyl alcohol, and simultaneously starting stirring; the mass ratio of the solid obtained by separating the materials in the elution kettle to the absolute ethyl alcohol is 1:3, a step of; repeating for 2 times;
4) Then carrying out solid-liquid separation to obtain absolute ethyl alcohol in which water-soluble saponin is dissolved; concentrating and crystallizing the absolute ethyl alcohol dissolved with the water-soluble saponin to obtain the water-soluble saponin, condensing and recycling the concentrated and separated absolute ethyl alcohol, and returning the concentrated and separated absolute ethyl alcohol to the step 3) for repeated use; and (3) mixing the petroleum ether solvent with dissolved saponin obtained by liquid separation with petroleum ether solvent with washing acid, neutralizing, concentrating and crystallizing to obtain oil-soluble saponin, condensing and recovering the concentrated and separated petroleum ether solvent, and returning to the step (1) for extracting the saponin or the step (2) for washing acid. The total yield of saponin in this example was 5.3%.
Example 6
1) The plant parts are subjected to alcohol extraction to obtain saponin extract, and acid is directly added into the saponin extract for hydrolysis; the mass ratio of the saponin extract to the sulfuric acid (calculated by the amount of pure sulfuric acid) is 1:0.4 to 0.8;
2) Directly carrying out solid-liquid separation after the step 1) is completed to obtain solid and acid liquor dissolved with water-soluble saponin; after the solid is dried, petroleum ether solvent is used for eluting oil-soluble partial saponin; the acid liquor dissolved with the water-soluble saponin is also washed for 1 time by using petroleum ether solvent and then returned to the step 1) for repeated use, and the volume ratio of the acid liquor to the total petroleum ether solvent for washing is 10:1, a step of;
3) Adding the solid after eluting the oil-soluble saponin into an elution kettle preloaded with absolute ethyl alcohol, and simultaneously starting stirring; the mass ratio of the solid obtained by separating the materials in the elution kettle to the absolute ethyl alcohol is 1:3, a step of; repeating for 2 times;
4) Then carrying out solid-liquid separation to obtain absolute ethyl alcohol in which water-soluble saponin is dissolved; concentrating and crystallizing the absolute ethyl alcohol dissolved with the water-soluble saponin to obtain the water-soluble saponin, condensing and recycling the concentrated and separated absolute ethyl alcohol, and returning the concentrated and separated absolute ethyl alcohol to the step 3) for repeated use; and (2) mixing the petroleum ether solvent dissolved with the saponin obtained by eluting the solid in the step (2) with the petroleum ether solvent of the washing acid, neutralizing, concentrating and crystallizing to obtain the oil-soluble saponin, condensing and recovering the petroleum ether solvent which is concentrated and separated, and returning to the step (2) for eluting the saponin or washing acid. The total yield of saponin in this example was 5.4%.
While the preferred embodiments of the present patent have been described in detail, the present patent is not limited to the above embodiments, and various changes may be made without departing from the spirit of the present patent within the knowledge of those skilled in the art. The foregoing is merely a preferred embodiment of the present application and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present application, which are intended to be comprehended within the scope of the present application.
Claims (1)
1. The extraction process of the water-soluble saponin is characterized by comprising the following steps:
1) The plant part adopts an alcohol extraction process to obtain a saponin extract, and acid liquor and petroleum ether solvent are simultaneously added into the saponin extract to carry out saponin extraction while hydrolyzing; the mass ratio of the saponin extract to the petroleum ether solvent to the acid solution is 1:1.4:0.6;
2) Separating out solid, petroleum ether solvent and acid solution dissolved with water-soluble saponin by using a three-phase separator after the step 1) is completed, washing the acid solution dissolved with water-soluble saponin by using petroleum ether solvent for 2 times, and returning the acid solution to the step 1) for repeated use so as to continuously improve the concentration of the water-soluble saponin in the acid solution, wherein the volume ratio of the acid solution dissolved with water-soluble saponin to the total amount of the petroleum ether solvent for washing is 10:2;
3) Drying the solid obtained by separating the materials, adding the dried solid into an elution kettle preloaded with absolute ethyl alcohol, and simultaneously starting stirring; the mass ratio of the solid obtained by separating the materials to the absolute ethyl alcohol is 1:5, a step of; repeating for 3 times;
4) Then carrying out solid-liquid separation to obtain absolute ethyl alcohol in which water-soluble saponin is dissolved; concentrating and crystallizing the absolute ethyl alcohol dissolved with the water-soluble saponin to obtain the water-soluble saponin, condensing and recycling the concentrated and separated absolute ethyl alcohol, and returning the concentrated and separated absolute ethyl alcohol to the step 3) for repeated use;
the plant part is Curcuma rhizome, rhizoma Dioscoreae Bulbiferae or semen Trigonellae.
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| GB702072A (en) * | 1951-04-02 | 1954-01-06 | Nat Res Dev | Improvements in or relating to the production of hecogenin from plant material |
| GB1056388A (en) * | 1964-04-23 | 1967-01-25 | Yves Rocher | Therapeutically useful ranunculus extracts |
| CN1274709C (en) * | 2004-11-23 | 2006-09-13 | 华中师范大学 | Saponin industry cleaning production technology |
| CN100460419C (en) * | 2005-12-08 | 2009-02-11 | 王喜军 | New cleanproduction process for extracting saponin from dioscorea zingiberensis |
| CN103319564A (en) * | 2013-06-24 | 2013-09-25 | 向华 | Method for producing diosgenin, yellow pigment and acidic starch by using yellow ginger |
| CN104844683B (en) * | 2015-04-15 | 2016-10-05 | 芜湖市丹洋现代农业科技发展有限公司 | A kind of method extracting tree peony saponin from the peony seeds dregs of rice |
| CN109438546A (en) * | 2018-10-23 | 2019-03-08 | 王吟箫 | A kind of technique that saponin is extracted from plants |
| CN109851656A (en) * | 2019-04-03 | 2019-06-07 | 山东洲星生物技术有限公司 | The technique of pigment and saponin is extracted in a kind of yellow ginger saponin(e |
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