CN111943991A - Extraction process of water-soluble saponin - Google Patents
Extraction process of water-soluble saponin Download PDFInfo
- Publication number
- CN111943991A CN111943991A CN201910402468.6A CN201910402468A CN111943991A CN 111943991 A CN111943991 A CN 111943991A CN 201910402468 A CN201910402468 A CN 201910402468A CN 111943991 A CN111943991 A CN 111943991A
- Authority
- CN
- China
- Prior art keywords
- saponin
- water
- soluble
- petroleum ether
- solid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000001397 quillaja saponaria molina bark Substances 0.000 title claims abstract description 192
- 229930182490 saponin Natural products 0.000 title claims abstract description 192
- 150000007949 saponins Chemical class 0.000 title claims abstract description 191
- 238000000605 extraction Methods 0.000 title claims abstract description 23
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 146
- 239000002253 acid Substances 0.000 claims abstract description 87
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 78
- 239000003208 petroleum Substances 0.000 claims abstract description 73
- 239000002904 solvent Substances 0.000 claims abstract description 73
- 239000007787 solid Substances 0.000 claims abstract description 54
- 238000000926 separation method Methods 0.000 claims abstract description 43
- 239000007788 liquid Substances 0.000 claims abstract description 36
- 239000000463 material Substances 0.000 claims abstract description 28
- 235000019441 ethanol Nutrition 0.000 claims abstract description 13
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims description 31
- 238000010828 elution Methods 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 16
- 230000008569 process Effects 0.000 claims description 13
- 230000003301 hydrolyzing effect Effects 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000003825 pressing Methods 0.000 claims description 4
- 150000002772 monosaccharides Chemical class 0.000 claims description 2
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 5
- 230000007062 hydrolysis Effects 0.000 abstract description 3
- 238000010364 biochemical engineering Methods 0.000 abstract description 2
- 238000002425 crystallisation Methods 0.000 abstract 1
- 230000008025 crystallization Effects 0.000 abstract 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 24
- 241000196324 Embryophyta Species 0.000 description 15
- WQLVFSAGQJTQCK-UHFFFAOYSA-N diosgenin Natural products CC1C(C2(CCC3C4(C)CCC(O)CC4=CCC3C2C2)C)C2OC11CCC(C)CO1 WQLVFSAGQJTQCK-UHFFFAOYSA-N 0.000 description 13
- 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 12
- 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 11
- 239000002351 wastewater Substances 0.000 description 11
- 238000002156 mixing Methods 0.000 description 7
- 230000003472 neutralizing effect Effects 0.000 description 6
- 241000908494 Dioscorea nipponica Species 0.000 description 5
- 235000017008 Dioscorea nipponica Nutrition 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000011343 solid material Substances 0.000 description 5
- 239000002699 waste material Substances 0.000 description 5
- 244000062245 Hedychium flavescens Species 0.000 description 4
- VFLDPWHFBUODDF-FCXRPNKRSA-N curcumin Chemical compound 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 description 4
- 239000003814 drug Substances 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000004064 recycling Methods 0.000 description 4
- 239000003270 steroid hormone Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 244000163122 Curcuma domestica Species 0.000 description 2
- 244000281702 Dioscorea villosa Species 0.000 description 2
- 241001678283 Dioscorea zingiberensis Species 0.000 description 2
- 235000004360 Dioscorea zingiberensis Nutrition 0.000 description 2
- XLYOFNOQVPJJNP-ZSJDYOACSA-N Heavy water Chemical compound [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 2
- 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 2
- RTMWIZOXNKJHRE-UHFFFAOYSA-N Tigogenin Natural products CC1COC2CC(C)(OC12)C3CCC4C5CCC6CC(O)CCC6(C)C5CCC34C RTMWIZOXNKJHRE-UHFFFAOYSA-N 0.000 description 2
- 244000250129 Trigonella foenum graecum Species 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 235000004879 dioscorea Nutrition 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000003911 water pollution Methods 0.000 description 2
- 240000009087 Crescentia cujete Species 0.000 description 1
- 235000005983 Crescentia cujete Nutrition 0.000 description 1
- 235000014375 Curcuma Nutrition 0.000 description 1
- 235000003392 Curcuma domestica Nutrition 0.000 description 1
- 235000005903 Dioscorea Nutrition 0.000 description 1
- 235000000504 Dioscorea villosa Nutrition 0.000 description 1
- 235000009797 Lagenaria vulgaris Nutrition 0.000 description 1
- 241000361919 Metaphire sieboldi Species 0.000 description 1
- 108010009736 Protein Hydrolysates Proteins 0.000 description 1
- 235000001484 Trigonella foenum graecum Nutrition 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
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- -1 diosgenin saponin Chemical class 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000008570 general process Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 125000001483 monosaccharide substituent group Chemical group 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- NWMIYTWHUDFRPL-UHFFFAOYSA-N sapogenin Natural products COC(=O)C1(CO)C(O)CCC2(C)C1CCC3(C)C2CC=C4C5C(C)(O)C(C)CCC5(CCC34C)C(=O)O NWMIYTWHUDFRPL-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 235000001019 trigonella foenum-graecum Nutrition 0.000 description 1
- 238000011144 upstream manufacturing 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
An extraction process of water-soluble saponin, which belongs to the technical field of biochemical engineering. The preparation method is characterized by comprising the following preparation steps: adding acid solution and petroleum ether solvent into saponin extract obtained by alcohol extraction to carry out hydrolysis and saponin extraction; separating the materials to obtain solid, a petroleum ether solvent and an acid solution dissolved with water-soluble saponin, and directly returning the acid solution dissolved with the water-soluble saponin to the step 1) for reuse; eluting the solid obtained by material separation by using absolute ethyl alcohol; the absolute ethyl alcohol dissolved with the water-soluble saponin is obtained by solid-liquid separation, the water-soluble saponin is obtained by concentration and crystallization, and the absolute ethyl alcohol obtained by concentration and separation is returned to the step 3) for reuse after being condensed and recovered. The invention integrates the sequence of a plurality of steps, increases the separation of the water-soluble saponin and further improves the yield of the saponin.
Description
Technical Field
An extraction process of water-soluble saponin, which belongs to the technical field of biochemical engineering.
Background
The saponin, also called sapogenin and saponin, is white crystal or powder, has a melting point of 195-205 ℃, is insoluble in water, is soluble in organic solvents such as benzene and chloroform, and is a basic raw material for producing steroid hormone medicines. The plant saponin mainly comprises three major types, namely diosgenin, tigogenin and tigogenin, wherein the diosgenin is the most ideal basic raw material for producing steroid hormone medicaments, and over two thirds of the steroid hormone medicaments in the world are produced by taking the diosgenin as the basic raw material, so the diosgenin has an important position in the production of the steroid hormone medicaments. The plant resources with high diosgenin content are few in the world and are mainly distributed in China and Mexico, so China and Mexico are large countries for diosgenin production. In mexico, plants with high diosgenin content are mainly scion-like dioscorea. In China, seventeen plants containing diosgenin exist, but the plants with high content and industrial development value mainly comprise yellow ginger, common yam rhizome and common fenugreek rhizome. The diosgenin content of the dioscorea nipponica is only half of that of the dioscorea zingiberensis (the saponin content of the dried dioscorea nipponica is about 2.5 percent, and the saponin content of the dioscorea nipponica is 1.2 percent), the growth cycle is longer than that of the dioscorea zingiberensis (the saponin content of the dioscorea nipponica is 2 years, and the saponin content of the Chinese fenugreek seeds is also lower (0.8 percent to 1.2 percent), and therefore, the dioscorea nipponica becomes the most main medicinal.
The traditional general process steps for extracting saponin from yellow ginger and rhizoma dioscoreae nipponicae comprise: pulverizing Curcuma rhizome, extracting with solvent to obtain saponin, hydrolyzing with acid, washing with water, oven drying to obtain hydrolysate, adding solvent, and performing solid-liquid separation to obtain liquid saponin. The pollution existing in the traditional process is mainly water pollution, and serious threat is formed to the protection of heavy water sources, and according to the production statistics of artificially planted yellow gingers, 130-180 tons of fresh yellow gingers and 15-20 tons of industrial hydrochloric acid (35%) are required for producing 1 ton of saponin in the traditional process, and 500 tons of wastewater is averagely discharged. In addition, about 10 tons of waste yellow ginger residues are discharged when 1 ton of saponin is produced. The average COD content in the comprehensive waste water of the diosgenin saponin is 25000 mg/L, the discharge amount of waste water and COD in the pharmaceutical and chemical industry which takes the saponin as a raw material accounts for about 8 percent of the total amount of China, the demand of the saponin in the international market is increased at a speed of not less than 6 percent every year, and the annual increase of China is higher than 10 percent, so the threat of water pollution of the saponin industry and downstream products thereof to the water environment is not ignored. Particularly, the high-yield areas of the diosgenin are positioned at the upstream of the central line water source Hanjiang of North-south-Water province, which is a water resource mainly protected in China, in Hubei, Shaanxi, Henan and other provinces, and in recent years, the COD discharge amount of the diosgenin waste water in the Hubei and Shaanxi provinces accounts for about 10 percent of the industrial COD discharge amount of the whole province, so that the amount and the urgency of pollution control on the water of the saponin industry are increased. The saponin production wastewater belongs to acid-containing high-concentration organic wastewater and is characterized in that: 1) poor biodegradability: BOD: 8000 mg/L; BOD/COD is about 0.27; the sugar content is high: the total sugar content of the comprehensive wastewater is about 2 percent, wherein most of the total sugar content is monosaccharide; pollution load: COD: 2-3 ten thousand mg/L (comprehensive wastewater); wherein the first liquid (about 20% of the wastewater, COD110000 mg/L); high acidity: pH: 1.0 to 2.5; high salt content: in wastewater at pH 1.0; cl-: 9600 mg/L (HCl hydrolysis process); SO (SO)4 2-：9300 mg/L （H2SO4A hydrolysis process). These salts remain (Cl) after neutralization-) Or remain (SO) for the most part4 2-). The ammonia nitrogen pollution exists, and the concentration is about 500 mg/L. The concentration of the pigment is about 3500 times.
In addition, the plant contains a large amount of water-soluble saponin besides the oil-soluble saponin which can be extracted by the traditional process, and the water-soluble saponin is not extracted and is attached to a solid byproduct or dissolved in waste acid to be discarded. The extraction rate of saponin cannot be further increased.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: overcomes the defects of the prior art and provides an extraction process of water-soluble saponin with high extraction rate.
The technical scheme adopted by the invention for solving the technical problems is as follows: the extraction process of the water-soluble saponin is characterized by comprising the following preparation steps:
1) extracting plant parts with alcohol to obtain saponin extract, and hydrolyzing with acid solution and petroleum ether solvent while extracting saponin;
2) separating materials after the step 1) is finished, separating the materials to obtain solid, a petroleum ether solvent and an acid solution dissolved with water-soluble saponin, and directly returning the acid solution dissolved with the water-soluble saponin to the step 1) for repeated use so as to continuously improve the concentration of the water-soluble saponin in the acid solution;
3) drying the solid obtained by material separation, adding the dried solid into an elution kettle pre-filled with anhydrous ethanol, and simultaneously starting stirring;
4) then carrying out solid-liquid separation to obtain absolute ethyl alcohol dissolved with water-soluble saponin; concentrating and crystallizing the absolute ethyl alcohol dissolved with the water-soluble saponin to obtain the water-soluble saponin, condensing and recovering the concentrated and separated absolute ethyl alcohol, and returning the condensed and separated absolute ethyl alcohol to the step 3) for reuse.
In the conventional preparation process, water-soluble saponin is generally attached to a solid byproduct or dissolved in waste acid to be discarded. The inventor of the invention realizes the recycling of waste acid in the early invention technology, thereby realizing the continuous enrichment of water-soluble saponin. Then mixing petroleum ether and acid liquor to extract water-soluble saponin with high concentration of water-soluble saponin. This method can extract part of water-soluble saponin, so as to increase the yield of saponin. But this approach is inefficient. However, because the solubility of the water-soluble saponin in the acid solution is relatively high, how to conveniently extract and separate the water-soluble saponin dissolved in the acid solution becomes a new technical bottleneck encountered by the inventor. In the invention, the inventor changes the idea, takes the separated solid as the breakthrough, and the concentration of the water-soluble saponin in the acid liquor is continuously improved on the basis of recycling the acid liquor. The inventor uses the original existing solid as the adsorption material, because the concentration of the water-soluble saponin in the acid solution is higher, part of the water-soluble saponin is inevitably adsorbed on the solid material in the hydrolysis reaction process, and the inventor uses the solid material as a breakthrough to wash out and separate the water-soluble saponin by adopting a solid material washing mode of absolute ethyl alcohol, thereby further improving the total yield of the saponin.
Preferably, the mass ratio of the saponin extract, the petroleum ether solvent and the acid in the step 1) is 1: 1.3-1.6: 0.4 to 0.8.
Preferably, the acid solution dissolved with the water-soluble saponin in the step 2) is washed by a petroleum ether solvent and then returned to the step 1), the washing times of the acid solution by the petroleum ether solvent are 1-3 times, and the volume ratio of the total amount of the acid solution to the petroleum ether solvent for washing is 10: 1 to 3. Washing with petroleum ether to extract and separate saponin as much as possible.
Preferably, the material separation is to directly separate solid, petroleum ether solvent and acid liquor dissolved with water-soluble saponin by using a three-phase separator.
Preferably, the material separation comprises the steps of carrying out solid-liquid separation through filter pressing to obtain a solid and a liquid, and then carrying out standing and liquid separation on the liquid to obtain a petroleum ether solvent and an acid solution dissolved with the water-soluble saponin.
The two material separation modes can meet the process requirements of the invention.
Preferably, the mass ratio of the solid obtained by separating the materials in the elution kettle to the absolute ethyl alcohol is 1: 3 to 6. The mass ratio can wash out the water-soluble saponin in the solid more thoroughly without consuming excessive ethanol.
Preferably, the step 3) is repeated for 2 to 4 times. The water-soluble saponin is washed more thoroughly after repeated washing.
The extraction process of the water-soluble saponin is characterized by comprising the following preparation steps:
1) extracting plant parts with alcohol to obtain saponin extract, and hydrolyzing with acid;
2) directly carrying out solid-liquid separation after the step 1) is finished to obtain solid and acid liquor dissolved with water-soluble saponin; after drying the solid, eluting oil-soluble partial saponin by using a petroleum ether solvent;
3) adding the solid after eluting the oil soluble saponin into an elution kettle pre-filled with anhydrous ethanol, and simultaneously starting stirring;
4) then carrying out solid-liquid separation to obtain monosaccharide massecuite and absolute ethyl alcohol dissolved with water-soluble saponin; concentrating and crystallizing the absolute ethyl alcohol dissolved with the water-soluble saponin to obtain the water-soluble saponin, condensing and recovering the concentrated and separated absolute ethyl alcohol, and returning the condensed and separated absolute ethyl alcohol to the step 3) for reuse.
Preferably, the petroleum ether solvent is concentrated and crystallized after the oil-soluble partial saponin is eluted to obtain the oil-soluble saponin, and the concentrated and separated petroleum ether solvent is condensed and recovered and then returned to the step 2) for reuse.
The plant parts in the process are the common turmeric, Chuanlong earthworm and calabash in the industry.
Compared with the prior art, the extraction process of the water-soluble saponin has the beneficial effects that: according to the preparation method, after the alcohol extraction step in the traditional process, a plurality of steps are integrated, the acid separated in the step 2) contains a small amount of water-soluble saponin, but the water-soluble saponin and the acid return to the step 1) in the process, so that the waste of discharge is avoided, and the extraction rate of the saponin can be effectively improved. The invention realizes the saponin production without wastewater discharge, the acid and the petroleum ether solvent are in a closed recycling state, no other loss is caused except trace residue in the separated solid in the process, the water consumption and the acid consumption are greatly saved, and the produced solid can be used subsequently, such as being used as feed. In the invention, the inventor changes the idea, takes the separated solid as the breakthrough, and the concentration of the water-soluble saponin in the acid liquor is continuously improved on the basis of recycling the acid liquor. The inventor uses the original existing solid as the adsorption material, because the concentration of the water-soluble saponin in the acid solution is higher, part of the water-soluble saponin is inevitably adsorbed on the solid material in the hydrolysis reaction process, and the inventor uses the method as a breakthrough to wash the solid material by absolute ethyl alcohol to wash and separate the water-soluble saponin, thereby further improving the total yield of the saponin.
Detailed Description
The invention is further illustrated by the following specific examples, of which example 1 is the best mode of practice.
Example 1
1) Extracting plant parts with alcohol to obtain saponin extract, and hydrolyzing with acid solution and petroleum ether solvent while extracting saponin; the mass ratio of the saponin extract to the petroleum ether solvent to the sulfuric acid (calculated by the pure sulfuric acid) is 1: 1.4: 0.6;
2) separating solid, petroleum ether solvent and acid liquor dissolved with water-soluble saponin from the finished product of the step 1) by using a three-phase separator, washing the acid liquor dissolved with the water-soluble saponin for 2 times by using the petroleum ether solvent, and returning 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 total amount of the acid liquor to the petroleum ether solvent for washing is 10: 2;
3) drying the solid obtained by material separation, adding the dried solid into an elution kettle pre-filled with anhydrous ethanol, and simultaneously starting stirring; the mass ratio of solid obtained by separating materials in the elution kettle to absolute ethyl alcohol is 1: 5; repeating the steps for 3 times;
4) then carrying out solid-liquid separation to obtain absolute ethyl alcohol dissolved with water-soluble saponin; concentrating and crystallizing the absolute ethyl alcohol dissolved with the water-soluble saponin to obtain the water-soluble saponin, condensing and recovering the concentrated and separated absolute ethyl alcohol, and returning the condensed and separated absolute ethyl alcohol to the step 3) for reuse; mixing the petroleum ether solvent with dissolved saponin obtained by liquid separation with the petroleum ether solvent of 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 saponin or returning to the step 2) for washing acid. The total yield of saponin in this example was 5.6%.
Example 2
1) Extracting plant parts with alcohol to obtain saponin extract, and hydrolyzing with acid solution and petroleum ether solvent while extracting saponin; the mass ratio of the saponin extract to the petroleum ether solvent to the sulfuric acid (calculated by the pure sulfuric acid) is 1: 1.5: 0.5;
2) separating solid, petroleum ether solvent and acid liquor dissolved with water-soluble saponin from the finished product of the step 1) by using a three-phase separator, washing the acid liquor dissolved with the water-soluble saponin for 2 times by using the petroleum ether solvent, and returning 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 total amount of the acid liquor to the petroleum ether solvent for washing is 10: 2.5;
3) drying the solid obtained by material separation, adding the dried solid into an elution kettle pre-filled with anhydrous ethanol, and simultaneously starting stirring; the mass ratio of solid obtained by separating materials in the elution kettle to absolute ethyl alcohol is 1: 4; repeating the steps for 3 times;
4) then carrying out solid-liquid separation to obtain absolute ethyl alcohol dissolved with water-soluble saponin; concentrating and crystallizing the absolute ethyl alcohol dissolved with the water-soluble saponin to obtain the water-soluble saponin, condensing and recovering the concentrated and separated absolute ethyl alcohol, and returning the condensed and separated absolute ethyl alcohol to the step 3) for reuse; mixing the petroleum ether solvent with dissolved saponin obtained by liquid separation with the petroleum ether solvent of 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 saponin or returning to the step 2) for washing acid. The total yield of saponin in this example was 5.5%.
Example 3
1) Extracting plant parts with alcohol to obtain saponin extract, and hydrolyzing with acid solution and petroleum ether solvent while extracting saponin; the mass ratio of the saponin extract to the petroleum ether solvent to the sulfuric acid (calculated by the pure sulfuric acid) is 1: 1.4: 0.7;
2) after the step 1) is finished, performing solid-liquid separation through filter pressing to separate the solid and the liquid into a solid phase and a liquid phase, then performing standing and liquid separation on the liquid phase to obtain a petroleum ether solvent and an acid solution in which water-soluble saponin is dissolved, washing the acid solution in which the water-soluble saponin is dissolved for 1-3 times by using the petroleum ether solvent, and returning 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 total amount of the acid solution to the petroleum ether solvent for: 1.5;
3) drying the solid obtained by material separation, adding the dried solid into an elution kettle pre-filled with anhydrous ethanol, and simultaneously starting stirring; the mass ratio of solid obtained by separating materials in the elution kettle to absolute ethyl alcohol is 1: 3.5; repeating the steps for 3 times;
4) then carrying out solid-liquid separation to obtain absolute ethyl alcohol dissolved with water-soluble saponin; concentrating and crystallizing the absolute ethyl alcohol dissolved with the water-soluble saponin to obtain the water-soluble saponin, condensing and recovering the concentrated and separated absolute ethyl alcohol, and returning the condensed and separated absolute ethyl alcohol to the step 3) for reuse; mixing the petroleum ether solvent with dissolved saponin obtained by liquid separation with the petroleum ether solvent of 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 saponin or returning to the step 2) for washing acid. The total yield of saponin in this example was 5.5%.
Example 4
1) Extracting plant parts with alcohol to obtain saponin extract, and hydrolyzing with acid solution and petroleum ether solvent while extracting saponin; the mass ratio of the saponin extract to the petroleum ether solvent to the sulfuric acid (calculated by the pure sulfuric acid) is 1: 1.6: 0.4;
2) separating solid, petroleum ether solvent and acid liquor dissolved with water-soluble saponin from the finished product of the step 1) by using a three-phase separator, washing the acid liquor dissolved with the water-soluble saponin for 3 times by using the petroleum ether solvent, and returning 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 total amount of the acid liquor to the petroleum ether solvent for washing is 10: 3;
3) drying the solid obtained by material separation, adding the dried solid into an elution kettle pre-filled with anhydrous ethanol, and simultaneously starting stirring; the mass ratio of solid obtained by separating materials in the elution kettle to absolute ethyl alcohol is 1: 6; repeating the steps for 4 times;
4) then carrying out solid-liquid separation to obtain absolute ethyl alcohol dissolved with water-soluble saponin; concentrating and crystallizing the absolute ethyl alcohol dissolved with the water-soluble saponin to obtain the water-soluble saponin, condensing and recovering the concentrated and separated absolute ethyl alcohol, and returning the condensed and separated absolute ethyl alcohol to the step 3) for reuse; mixing the petroleum ether solvent with dissolved saponin obtained by liquid separation with the petroleum ether solvent of 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 saponin or returning to the step 2) for washing acid. The total yield of saponin in this example was 5.3%.
Example 5
1) Extracting plant parts with alcohol to obtain saponin extract, and hydrolyzing with acid solution and petroleum ether solvent while extracting saponin; the mass ratio of the saponin extract to the petroleum ether solvent to the sulfuric acid (calculated by the pure sulfuric acid) is 1: 1.3: 0.8;
2) after the step 1) is finished, performing solid-liquid separation through filter pressing to separate the solid and the liquid into a solid phase and a liquid phase, then performing standing and liquid separation on the liquid phase to obtain a petroleum ether solvent and an acid solution dissolved with water-soluble saponin, washing the acid solution dissolved with the water-soluble saponin for 1 time by using the petroleum ether solvent, and returning 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 total amount of the petroleum ether solvent for the acid solution and washing is 10: 1;
3) drying the solid obtained by material separation, adding the dried solid into an elution kettle pre-filled with anhydrous ethanol, and simultaneously starting stirring; the mass ratio of solid obtained by separating materials in the elution kettle to absolute ethyl alcohol is 1: 3; repeating the steps for 2 times;
4) then carrying out solid-liquid separation to obtain absolute ethyl alcohol dissolved with water-soluble saponin; concentrating and crystallizing the absolute ethyl alcohol dissolved with the water-soluble saponin to obtain the water-soluble saponin, condensing and recovering the concentrated and separated absolute ethyl alcohol, and returning the condensed and separated absolute ethyl alcohol to the step 3) for reuse; mixing the petroleum ether solvent with dissolved saponin obtained by liquid separation with the petroleum ether solvent of 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 saponin or returning to the step 2) for washing acid. The total yield of saponin in this example was 5.3%.
Example 6
1) Extracting plant parts with alcohol to obtain saponin extract, and hydrolyzing with acid; the mass ratio of the saponin extract to the sulfuric acid (calculated by the pure sulfuric acid) is 1: 0.4 to 0.8;
2) directly carrying out solid-liquid separation after the step 1) is finished to obtain solid and acid liquor dissolved with water-soluble saponin; after drying the solid, eluting oil-soluble partial saponin by using a petroleum ether solvent; washing the acid solution dissolved with the water-soluble saponin for 1 time by using a petroleum ether solvent, and returning the acid solution to the step 1) for repeated use, wherein the volume ratio of the total amount of the acid solution to the petroleum ether solvent for washing is 10: 1;
3) adding the solid after eluting the oil soluble saponin into an elution kettle pre-filled with anhydrous ethanol, and simultaneously starting stirring; the mass ratio of solid obtained by separating materials in the elution kettle to absolute ethyl alcohol is 1: 3; repeating the steps for 2 times;
4) then carrying out solid-liquid separation to obtain absolute ethyl alcohol dissolved with water-soluble saponin; concentrating and crystallizing the absolute ethyl alcohol dissolved with the water-soluble saponin to obtain the water-soluble saponin, condensing and recovering the concentrated and separated absolute ethyl alcohol, and returning the condensed and separated absolute ethyl alcohol to the step 3) for reuse; mixing the petroleum ether solvent with dissolved saponin obtained by eluting the solid in the step 2) and the petroleum ether solvent of the 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 2) to elute the saponin or wash the acid. The total yield of saponin in this example was 5.4%.
The foregoing is directed to preferred embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.
Claims (9)
1. The extraction process of the water-soluble saponin is characterized by comprising the following preparation steps:
1) extracting plant parts with alcohol to obtain saponin extract, and hydrolyzing with acid solution and petroleum ether solvent while extracting saponin;
2) separating materials after the step 1) is finished, separating the materials to obtain solid, a petroleum ether solvent and an acid solution dissolved with water-soluble saponin, and directly returning the acid solution dissolved with the water-soluble saponin to the step 1) for repeated use so as to continuously improve the concentration of the water-soluble saponin in the acid solution;
3) drying the solid obtained by material separation, adding the dried solid into an elution kettle pre-filled with anhydrous ethanol, and simultaneously starting stirring;
4) then carrying out solid-liquid separation to obtain absolute ethyl alcohol dissolved with water-soluble saponin; concentrating and crystallizing the absolute ethyl alcohol dissolved with the water-soluble saponin to obtain the water-soluble saponin, condensing and recovering the concentrated and separated absolute ethyl alcohol, and returning the condensed and separated absolute ethyl alcohol to the step 3) for reuse.
2. The extraction process of water-soluble saponin as claimed in claim 1, wherein: the mass ratio of the saponin extract, the petroleum ether solvent and the acid in the step 1) is 1: 1.3-1.6: 0.4 to 0.8.
3. The extraction process of water-soluble saponin as claimed in claim 1, wherein: washing the acid solution dissolved with the water-soluble saponin in the step 2) by using a petroleum ether solvent, and returning to the step 1), wherein the washing times of the acid solution by using the petroleum ether solvent are 1-3 times, and the volume ratio of the total amount of the acid solution to the petroleum ether solvent for washing is 10: 1 to 3.
4. The extraction process of water-soluble saponin as claimed in claim 1, wherein: the material separation is to directly separate solid, petroleum ether solvent and acid liquor dissolved with water-soluble saponin by using a three-phase separator.
5. The extraction process of water-soluble saponin as claimed in claim 1, wherein: the material separation comprises the steps of carrying out solid-liquid separation through filter pressing to obtain a solid and a liquid, and then carrying out standing and liquid separation on the liquid to obtain a petroleum ether solvent and an acid solution dissolved with water-soluble saponin.
6. The extraction process of water-soluble saponin as claimed in claim 1, wherein: the mass ratio of the solid obtained by separating the materials in the elution kettle to the absolute ethyl alcohol is 1: 3 to 6.
7. The extraction process of water-soluble saponin as claimed in claim 1, wherein: and the step 3) is repeated for 2-4 times.
8. The extraction process of the water-soluble saponin is characterized by comprising the following preparation steps:
1) extracting plant parts with alcohol to obtain saponin extract, and hydrolyzing with acid;
2) directly carrying out solid-liquid separation after the step 1) is finished to obtain solid and acid liquor dissolved with water-soluble saponin; after drying the solid, eluting oil-soluble partial saponin by using a petroleum ether solvent;
3) adding the solid after eluting the oil soluble saponin into an elution kettle pre-filled with anhydrous ethanol, and simultaneously starting stirring;
4) then carrying out solid-liquid separation to obtain monosaccharide massecuite and absolute ethyl alcohol dissolved with water-soluble saponin; concentrating and crystallizing the absolute ethyl alcohol dissolved with the water-soluble saponin to obtain the water-soluble saponin, condensing and recovering the concentrated and separated absolute ethyl alcohol, and returning the condensed and separated absolute ethyl alcohol to the step 3) for reuse.
9. The process of claim 8, wherein the extraction of water soluble saponin comprises: the petroleum ether solvent is concentrated and crystallized after eluting the oil-soluble partial saponin to obtain the oil-soluble saponin, and the concentrated and separated petroleum ether solvent is condensed and recovered and then returned to the step 2) for reuse.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910402468.6A CN111943991A (en) | 2019-05-15 | 2019-05-15 | Extraction process of water-soluble saponin |
| CN202310746277.8A CN116789715A (en) | 2019-05-15 | 2019-05-15 | Extraction process of water-soluble saponin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910402468.6A CN111943991A (en) | 2019-05-15 | 2019-05-15 | Extraction process of water-soluble saponin |
Related Child Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310746277.8A Division CN116789715A (en) | 2019-05-15 | 2019-05-15 | Extraction process of water-soluble saponin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111943991A true CN111943991A (en) | 2020-11-17 |
Family
ID=73336360
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310746277.8A Pending CN116789715A (en) | 2019-05-15 | 2019-05-15 | Extraction process of water-soluble saponin |
| CN201910402468.6A Pending CN111943991A (en) | 2019-05-15 | 2019-05-15 | Extraction process of water-soluble saponin |
Family Applications Before (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310746277.8A Pending CN116789715A (en) | 2019-05-15 | 2019-05-15 | Extraction process of water-soluble saponin |
Country Status (1)
| Country | Link |
|---|---|
| CN (2) | CN116789715A (en) |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB702072A (en) * | 1951-04-02 | 1954-01-06 | Nat Res Dev | Improvements in or relating to the production of hecogenin from plant material |
| US3464972A (en) * | 1964-04-23 | 1969-09-02 | Yves Rocher | Method of extracting saponins |
| CN1651445A (en) * | 2004-11-23 | 2005-08-10 | 华中师范大学 | Saponin industry cleaning production technology |
| CN1978458A (en) * | 2005-12-08 | 2007-06-13 | 王喜军 | New cleanproduction process for extracting saponin from dioscorea zingiberensis |
| CN104031114A (en) * | 2013-06-24 | 2014-09-10 | 向华 | Method for producing diosgenin, uranidin and acid starch by using yellow ginger |
| CN104844683A (en) * | 2015-04-15 | 2015-08-19 | 芜湖市丹洋现代农业科技发展有限公司 | Method for extracting peony saponin from peony seed meal |
| 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 |
-
2019
- 2019-05-15 CN CN202310746277.8A patent/CN116789715A/en active Pending
- 2019-05-15 CN CN201910402468.6A patent/CN111943991A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB702072A (en) * | 1951-04-02 | 1954-01-06 | Nat Res Dev | Improvements in or relating to the production of hecogenin from plant material |
| US3464972A (en) * | 1964-04-23 | 1969-09-02 | Yves Rocher | Method of extracting saponins |
| CN1651445A (en) * | 2004-11-23 | 2005-08-10 | 华中师范大学 | Saponin industry cleaning production technology |
| CN1978458A (en) * | 2005-12-08 | 2007-06-13 | 王喜军 | New cleanproduction process for extracting saponin from dioscorea zingiberensis |
| CN104031114A (en) * | 2013-06-24 | 2014-09-10 | 向华 | Method for producing diosgenin, uranidin and acid starch by using yellow ginger |
| CN104844683A (en) * | 2015-04-15 | 2015-08-19 | 芜湖市丹洋现代农业科技发展有限公司 | Method for extracting peony saponin from peony seed meal |
| 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 |
Non-Patent Citations (3)
| Title |
|---|
| 张友德主编: "《黄姜优质栽培新技术》", 30 September 2005, 金盾出版社 * |
| 杨铖 等: "黄姜渣提取淀粉的成分及颗粒结构分析", 《安徽农业科学》 * |
| 江苏省植物研究所 等编著: "《新华本草纲要》", 30 June 1988, 上海科学技术出版社 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN116789715A (en) | 2023-09-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104326981B (en) | A kind of high efficiency extraction separation method of bulleyaconitine A | |
| WO2020228786A1 (en) | Industrialized method for rapidly and efficiently extracting xanthophyll and quercetagetin | |
| CN101402669A (en) | Environment friendly method for producing diosgenin | |
| CN109053821B (en) | Method for extracting tea polyphenol, total amino acids and flavone compounds from momordica grosvenori leaves | |
| WO2020082527A1 (en) | Process for extracting saponin from plant | |
| CN112920034A (en) | Method for extracting 6-gingerol with content of more than or equal to 98% | |
| CN104945463A (en) | Extracting method for tea saponin | |
| CN103319565B (en) | Clean and high-efficiency process for producing diosgenin | |
| CN105985315A (en) | Method for extracting nicotine from tobacco waste | |
| CN108117571B (en) | Preparation method of gentiopicroside monomer | |
| CN111171104B (en) | Method for preparing ursolic acid from rosemary oil paste by-product | |
| CN111943991A (en) | Extraction process of water-soluble saponin | |
| CN101429197B (en) | Extraction method for joint production of coptis chinensis with coptis chinensis fibrous root as raw material | |
| CN110256189A (en) | The technique of lycopene is extracted from tomato peel | |
| CN102489036A (en) | Method for extracting lycopene by using continuous countercurrent ultrasonic extractor | |
| WO2020199410A1 (en) | Process for extracting pigment and saponin from turmeric | |
| CN108484423A (en) | A method of isolating and purifying l-Alanine from l-Alanine zymotic fluid | |
| CN1054788A (en) | Process for extracting grease and tea saponin by one-step leaching of cake dregs | |
| CN100393882C (en) | Galantamin hydrobromide production method | |
| CN112094184B (en) | Method for extracting shikimic acid from ginkgo leaf extract chromatographic wastewater | |
| CN107056605B (en) | Method for separating unsaturated fatty acid and phytosterol from gardner seed oil | |
| CN108774131B (en) | Method for separating and purifying cynarin and chlorogenic acid in artichoke by simulated moving bed chromatography | |
| CN101307086B (en) | Process for purifying 3beta-cholest-5,24-diene-3-alcohol y solvent crystallization method | |
| CN110790811A (en) | Method for preparing diosgenin by aluminum chloride hydrolysis in two-phase system | |
| CN105669419B (en) | The method of saccharic acid in sequential simulated moving bed separating corn stalk acid hydrolysis solution |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20201117 |