CN101591373A - A kind of extracting method of dioscin - Google Patents
A kind of extracting method of dioscin Download PDFInfo
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- CN101591373A CN101591373A CNA2008100498882A CN200810049888A CN101591373A CN 101591373 A CN101591373 A CN 101591373A CN A2008100498882 A CNA2008100498882 A CN A2008100498882A CN 200810049888 A CN200810049888 A CN 200810049888A CN 101591373 A CN101591373 A CN 101591373A
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- dioscin
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- HDXIQHTUNGFJIC-UHFFFAOYSA-N (25R)-spirost-5-en-3beta-ol 3-O-<O-alpha-L-rhamnopyranosyl-(1-->2)-beta-D-glucopyranoside> Natural products O1C2(OCC(C)CC2)C(C)C(C2(CCC3C4(C)CC5)C)C1CC2C3CC=C4CC5OC1OC(CO)C(O)C(O)C1OC1OC(C)C(O)C(O)C1O HDXIQHTUNGFJIC-UHFFFAOYSA-N 0.000 title claims abstract description 49
- VNONINPVFQTJOC-RXEYMUOJSA-N Collettiside III Natural products O([C@@H]1[C@@H](O)[C@H](O[C@H]2[C@H](O)[C@H](O)[C@@H](O)[C@H](C)O2)[C@H](CO)O[C@@H]1O[C@@H]1CC=2[C@@](C)([C@@H]3[C@H]([C@H]4[C@@](C)([C@H]5[C@H](C)[C@@]6(O[C@H]5C4)OC[C@H](C)CC6)CC3)CC=2)CC1)[C@H]1[C@H](O)[C@H](O)[C@@H](O)[C@H](C)O1 VNONINPVFQTJOC-RXEYMUOJSA-N 0.000 title claims abstract description 49
- VNONINPVFQTJOC-ZGXDEBHDSA-N dioscin Chemical compound O([C@@H]1[C@@H](CO)O[C@H]([C@@H]([C@H]1O)O[C@H]1[C@@H]([C@H](O)[C@@H](O)[C@H](C)O1)O)O[C@@H]1CC2=CC[C@H]3[C@@H]4C[C@H]5[C@@H]([C@]4(CC[C@@H]3[C@@]2(C)CC1)C)[C@@H]([C@]1(OC[C@H](C)CC1)O5)C)[C@@H]1O[C@@H](C)[C@H](O)[C@@H](O)[C@H]1O VNONINPVFQTJOC-ZGXDEBHDSA-N 0.000 title claims abstract description 49
- CJNUQCDDINHHHD-APRUHSSNSA-N dioscin Natural products C[C@@H]1CC[C@@]2(OC1)O[C@H]3C[C@H]4[C@@H]5CC=C6C[C@H](CC[C@@H]6[C@H]5CC[C@]4(C)[C@H]3[C@@H]2C)O[C@@H]7O[C@H](CO)[C@@H](O[C@@H]8O[C@@H](C)[C@H](O)[C@@H](O)[C@H]8O)[C@H](O)[C@H]7O[C@@H]9O[C@@H](C)[C@H](O)[C@@H](O)[C@H]9O CJNUQCDDINHHHD-APRUHSSNSA-N 0.000 title claims abstract description 49
- VNONINPVFQTJOC-UHFFFAOYSA-N polyphyllin III Natural products O1C2(OCC(C)CC2)C(C)C(C2(CCC3C4(C)CC5)C)C1CC2C3CC=C4CC5OC(C(C1O)OC2C(C(O)C(O)C(C)O2)O)OC(CO)C1OC1OC(C)C(O)C(O)C1O VNONINPVFQTJOC-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 47
- WQLVFSAGQJTQCK-UHFFFAOYSA-N diosgenin Natural products CC1C(C2(CCC3C4(C)CCC(O)CC4=CCC3C2C2)C)C2OC11CCC(C)CO1 WQLVFSAGQJTQCK-UHFFFAOYSA-N 0.000 claims abstract description 29
- DWCSNWXARWMZTG-UHFFFAOYSA-N Trigonegenin A Natural products CC1C(C2(CCC3C4(C)CCC(O)C=C4CCC3C2C2)C)C2OC11CCC(C)CO1 DWCSNWXARWMZTG-UHFFFAOYSA-N 0.000 claims abstract description 28
- 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 claims abstract description 28
- 239000000843 powder Substances 0.000 claims abstract description 16
- 239000002904 solvent Substances 0.000 claims abstract description 13
- 239000013543 active substance Substances 0.000 claims abstract description 12
- 239000007787 solid Substances 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000284 extract Substances 0.000 claims abstract description 6
- 239000004094 surface-active agent Substances 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 3
- 238000012216 screening Methods 0.000 claims abstract description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 9
- 241000196324 Embryophyta Species 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 230000007062 hydrolysis Effects 0.000 claims description 7
- 238000006460 hydrolysis reaction Methods 0.000 claims description 7
- 230000002378 acidificating effect Effects 0.000 claims description 4
- 239000003054 catalyst Substances 0.000 claims description 4
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 3
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 3
- 238000005238 degreasing Methods 0.000 claims description 3
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 3
- 244000144992 flock Species 0.000 claims description 3
- 238000001556 precipitation Methods 0.000 claims description 3
- 238000001953 recrystallisation Methods 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 3
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 3
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 2
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 2
- 241000244987 Daiswa polyphylla Species 0.000 claims description 2
- 239000004141 Sodium laurylsulphate Substances 0.000 claims description 2
- ZCZSIDMEHXZRLG-UHFFFAOYSA-N acetic acid heptyl ester Natural products CCCCCCCOC(C)=O ZCZSIDMEHXZRLG-UHFFFAOYSA-N 0.000 claims description 2
- IPBVNPXQWQGGJP-UHFFFAOYSA-N acetic acid phenyl ester Natural products CC(=O)OC1=CC=CC=C1 IPBVNPXQWQGGJP-UHFFFAOYSA-N 0.000 claims description 2
- 229940043232 butyl acetate Drugs 0.000 claims description 2
- 239000012141 concentrate Substances 0.000 claims description 2
- 150000002148 esters Chemical class 0.000 claims description 2
- 229940093499 ethyl acetate Drugs 0.000 claims description 2
- JPXGPRBLTIYFQG-UHFFFAOYSA-N heptan-4-yl acetate Chemical compound CCCC(CCC)OC(C)=O JPXGPRBLTIYFQG-UHFFFAOYSA-N 0.000 claims description 2
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 2
- 239000003456 ion exchange resin Substances 0.000 claims description 2
- 229920003303 ion-exchange polymer Polymers 0.000 claims description 2
- 229940049953 phenylacetate Drugs 0.000 claims description 2
- WLJVXDMOQOGPHL-UHFFFAOYSA-N phenylacetic acid Chemical compound OC(=O)CC1=CC=CC=C1 WLJVXDMOQOGPHL-UHFFFAOYSA-N 0.000 claims description 2
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 2
- 229920000053 polysorbate 80 Polymers 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 claims description 2
- 238000000605 extraction Methods 0.000 abstract description 22
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 abstract description 21
- 239000000243 solution Substances 0.000 abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 14
- 239000003960 organic solvent Substances 0.000 abstract description 10
- 239000007864 aqueous solution Substances 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 244000281702 Dioscorea villosa Species 0.000 description 6
- 235000004879 dioscorea Nutrition 0.000 description 6
- 235000002722 Dioscorea batatas Nutrition 0.000 description 5
- 235000006536 Dioscorea esculenta Nutrition 0.000 description 5
- 241000908494 Dioscorea nipponica Species 0.000 description 5
- 240000001811 Dioscorea oppositifolia Species 0.000 description 5
- 235000003416 Dioscorea oppositifolia Nutrition 0.000 description 5
- 244000062245 Hedychium flavescens Species 0.000 description 5
- 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 5
- 238000005303 weighing Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 235000017008 Dioscorea nipponica Nutrition 0.000 description 3
- 241000374766 Dioscorea panthaica Species 0.000 description 3
- 238000005903 acid hydrolysis reaction Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000001397 quillaja saponaria molina bark Substances 0.000 description 3
- 229930182490 saponin Natural products 0.000 description 3
- 150000007949 saponins Chemical class 0.000 description 3
- 235000009926 Dioscorea panthaica Nutrition 0.000 description 2
- 229920002472 Starch Polymers 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000003110 anti-inflammatory effect Effects 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000008107 starch Substances 0.000 description 2
- 235000019698 starch Nutrition 0.000 description 2
- 240000000530 Alcea rosea Species 0.000 description 1
- 235000017334 Alcea rosea Nutrition 0.000 description 1
- 235000017303 Althaea rosea Nutrition 0.000 description 1
- 241000505835 Deutzia hypoglauca Species 0.000 description 1
- 241000908131 Dioscorea gracillima Species 0.000 description 1
- 241000223674 Dioscorea parviflora Species 0.000 description 1
- 241001678283 Dioscorea zingiberensis Species 0.000 description 1
- 235000004360 Dioscorea zingiberensis Nutrition 0.000 description 1
- 206010018910 Haemolysis Diseases 0.000 description 1
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 description 1
- 238000000944 Soxhlet extraction Methods 0.000 description 1
- 239000003377 acid catalyst Substances 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 239000003433 contraceptive agent Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000008588 hemolysis Effects 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000035772 mutation Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000004064 recycling 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
- 239000003270 steroid hormone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Landscapes
- Extraction Or Liquid Replacement (AREA)
- Saccharide Compounds (AREA)
- Steroid Compounds (AREA)
Abstract
The present invention relates to a kind of extracting method of dioscin, may further comprise the steps: plant drying, crushing screening that (1) will contain dioscin get dry powder; (2) surfactant dissolves is mixed with solvent in water; (3) solvent that the dry powder and the step (2) of step (1) gained are prepared, the ratio of solvent and dry powder is 0.1: 1～100: 1, extracts with intensified by ultrasonic wave, isolates solid, can obtain containing the extracting solution of dioscin; (4) extracting solution is handled thick dioscin or thick diosgenin.Adopt the extracting method of organic solvent to compare with tradition, method of the present invention has avoided using organic solvents such as volatile methyl alcohol, ethanol fully, optimum extraction time by tens hours of traditional method foreshorten to the inventive method less than 20 minutes, and extraction yield has improved 4～5%.In addition, adopt the aqueous solution of tensio-active agent to leach, it is compared with employed methyl alcohol, ethanol in the prior art, and cost reduces greatly, and security is good, is specially adapted to industrialized production.
Description
Technical field
The present invention relates to a kind of extracting method of dioscin, relate in particular to a kind of method that adopts ultrasonic-water phase surfactant mixture to unite extraction dioscin from contain the dioscin plant.
Background technology
It is in the various plants of representative that dioscin (diocsin) is prevalent in the yam, has biological activitys such as anticancer, antibacterial, desinsection, anti-inflammatory, and in addition, dioscin is still produced the basic raw material of diosgenin (diosgenin).Diosgenin has another name called saponin, has multiple pharmacological effect such as haemolysis, reducing blood-fat, antibiotic, anti-inflammatory, can be used as the basic medicine chemical material of synthesizing steroid hormone medicine and contraceptive steroid, has important pharmacology and is worth and the vast market potentiality.China's diosgenin annual production at present surpasses 2000 tons, has become diosgenin producing country the biggest in the world.
China diosgenin enterprise generally adopts direct acid-hydrolysis method to produce, its step is produced diosgenin for directly inorganic acid (hydrochloric acid, sulfuric acid etc.) catalyzer and yellow ginger or Dioscorea nipponica Mak. Ningpo Yam Rhizome rhizome Hybrid Heating being hydrolyzed, in hydrolytic process, content is polluted, destroys and can't utilize by strong acid catalyst up to starch more than 90% (dry weight) and fiber etc. in yellow ginger or the Dioscorea nipponica Mak. Ningpo Yam Rhizome rhizome, the COD value is up to 30000mg/l in the waste discharge after the hydrolysis, and environmental pollution is very serious.For this reason, Many researchers is attempted at first dioscin being extracted acid hydrolysis again from plant and is produced diosgenin, to reduce with the acid amount, to alleviate environmental pollution, promotes the recycling of compositions such as starch, fiber.But in the currently used method of the extraction of dioscin mostly with an organic solvent the aqueous solution of (as methyl alcohol, ethanol etc.) or organic solvent leach, as application number is that 200510022745.9 the patent of invention and the patent No. are that 03144208.0 patent of invention all is to adopt methyl alcohol or ethanol to leach, shortcomings such as all there is extraction time long (a few hours to tens hour) in aforesaid method, solvent load is big, cost is high, energy consumption is high, efficient is low are not suitable for industrialized production; In addition, used organic solvent (as methyl alcohol, ethanol) is poisonous, volatile, and security is relatively poor.Be badly in need of at present a kind of efficiently, dioscin extracting method cheaply of exploitation.
Summary of the invention
The objective of the invention is to propose a kind of from contain the dioscin plant method of high efficiency extraction dioscin, its technological process is simple, cost is low, efficient is high.
To achieve these goals, technical scheme of the present invention has adopted a kind of extracting method of dioscin, specifically may further comprise the steps:
(1) will contain plant drying, the crushing screening of dioscin, dry powder; Usually be crushed to 50～100 orders;
(2) surfactant dissolves is mixed with solvent in water;
(3) solvent that the dry powder and the step (2) of step (1) gained are prepared, the ratio of solvent and dry powder is 0.1: 1～100: 1 (ml/g), extracts 0～120min with intensified by ultrasonic wave, can suitably heat during extraction, isolate solid, can obtain containing the extracting solution of dioscin;
(4) extracting solution is handled thick saponin(e or thick diosgenin.
Comprise that also thick dioscin from Paris polyphylla Smith is purified or diosgenin is produced in further processing.
Wherein the dioscin plant optimization that contains in the step (1) is: Rhizome of Peltate Yam (Dioscoreazingiberensis C.H.wright), Ningpo Yam Rhizome Chinese yam (D.nipponica Makino), Xiao Hua Chinese yam (D.parviflora Ting Sp.Nov), Dioscorea panthaica Prain et Burkill (D.Panthaica Prain et.Burk), bavin yellow ginger (D.nipponica Makno subsp.Deltoidea wall) and mutation thereof, very thin Chinese yam (D.gracillimaMiq.), hollyhock leaf (D.althacoides Knuth), powder back of the body Chinese yam (D.hypoglauca Palib).
Tensio-active agent in the described step (2) is any one or its combination in sodium lauryl sulphate, sodium laurylsulfonate, Sodium dodecylbenzene sulfonate, cetyl trimethylammonium bromide or the tween-80.
The massfraction of tensio-active agent is 1～50% in the solvent of described step (2) preparation.
Step (3) applies ultrasonic field and extracts to strengthen when extracting, wherein ultrasonic frequency range is 10～5000KHz.
The treatment process of the extracting solution of step (4) is: concentrate the back and add the skim soln degreasing, the separation concentrated solution evaporated under reduced pressure gets thick dioscin.Described skim soln is a low-molecular-weight ester, is preferably ethyl acetate, butylacetate, phenylacetate or heptyl acetate.
The treatment process of the extracting solution of step (4) is: be concentrated into flocks and separate out, collecting precipitation gets thick dioscin.
The treatment process of the extracting solution of step (4) is: directly add an acidic catalyst and heating hydrolysis in extracting solution, get thick diosgenin.
Described an acidic catalyst is any one in hydrochloric acid, sulfuric acid or the ion exchange resin.
The method of ultrasonic-water phase surfactant mixture associating that the present invention adopts is extracted dioscin from contain the dioscin plant, the adding of tensio-active agent can reduce the interfacial tension of solid-liquid phase, increase the dissolving of larger molecular organics in water and ooze out ability, shortened infiltrating time greatly, improve extraction yield, can replace traditional organic solvent; Ultrasonic because of its inherent mechanical effect, heat effect, hole effect etc., promoted tensio-active agent and water molecules in vegetable cell infiltration and dioscin to solution diffusion mutually, improved the extraction effect of tensio-active agent greatly.Adopt the extracting method of organic solvent to compare with tradition, method of the present invention has avoided using organic solvents such as volatile methyl alcohol, ethanol fully, optimum extraction time by tens hours of traditional method foreshorten to the inventive method less than 20 minutes, and extraction yield has improved 4～5%.In addition, adopt the aqueous solution of tensio-active agent to leach, it is compared with employed methyl alcohol, ethanol in the prior art, and cost reduces greatly, and security is good, is specially adapted to industrialized production.Adopt method of the present invention earlier dioscin to be extracted, and then the production diosgenin that is hydrolyzed, can significantly reduce measuring of sapogenin production like this with acid, alleviate environmental pollution, promote the comprehensive utilization of raw material, have good social benefit and economic benefit.
Embodiment
Embodiment 1
The method of present embodiment may further comprise the steps: 80 orders are cleaned, dry, are crushed to the Dioscorea nipponica Mak. Ningpo Yam Rhizome rhizome, take by weighing dry powder 5.00g, the adding massfraction is 3.0% lauryl sodium sulfate aqueous solution, liquid-solid ratio is that the ratio of solvent and dry powder is 8: 1, with frequency is that 20KHz, power are the supersound extraction 20min of 60W, and separate solid gets extracting solution; Add HCl and heating hydrolysis in extracting solution, get thick diosgenin, measuring gained diosgenin yield is 1.86%.
Embodiment 2
The method of present embodiment may further comprise the steps: 90 orders are cleaned, dry, are crushed to the yellow ginger rhizome, take by weighing dry powder 5.00g, the adding massfraction is 5.0% sodium dodecyl sulfate aqueous solution, liquid-solid ratio 12: 1, with frequency is that 30KHz, power are the supersound extraction 30min of 90W, and separate solid obtains extracting solution; Add sulfuric acid and heating hydrolysis in extracting solution, get thick diosgenin, measuring gained diosgenin yield is 1.88%.
Embodiment 3
The method of present embodiment may further comprise the steps: 100 orders are cleaned, dry, are crushed to very thin Chinese yam rhizome, take by weighing dry powder 5.00g, the adding massfraction is 7.0% sodium dodecyl benzene sulfonate aqueous solution, liquid-solid ratio 10: 1, with frequency is that 15KHz, power are the supersound extraction 10min of 120W, and separate solid obtains extracting solution; Separation concentrated solution after the degreasing of adding ethyl acetate after concentrating, evaporated under reduced pressure gets thick dioscin 0.21g.Thick dioscin adds sulfuric acid and heating hydrolysis, gets thick diosgenin, and recrystallization gets high purity diosgenin 0.091g, and measuring gained diosgenin yield is 1.82%.
Embodiment 4
The method of present embodiment may further comprise the steps: 70 orders are cleaned, dry, are crushed to the Dioscorea panthaica Prain et Burkill rhizome, take by weighing dry powder 5.00g, the adding massfraction is 4.0% the cetyl trimethylammonium bromide aqueous solution, liquid-solid ratio 16: 1, with frequency is that 20KHz, power are the supersound extraction 5min of 150W, and separate solid obtains extracting solution, extracting solution is concentrated into flocks separates out, collecting precipitation gets thick dioscin 0.17g.Thick dioscin adds sulfuric acid and heating hydrolysis, gets thick diosgenin, and recrystallization gets high purity diosgenin 0.089g, and measuring gained diosgenin yield is 1.78%.
Comparison with traditional method:
Take by weighing yellow ginger dry powder 5.00g and strengthen extraction method and tensio-active agent of the present invention-supersonic synergic extraction method (embodiment 2) with conventional organic solvents extraction, soxhlet extraction, tensio-active agent respectively, the dioscin and the acid hydrolysis of extracting wherein are diosgenin, relatively the extraction time and the extraction yield of the whole bag of tricks the results are shown in Table 1.
The comparison of the different extraction processes of table 1
Above result shows, of the present invention ultrasonic-tensio-active agent is collaborative to extract the use that the saponin(e method has been avoided a large amount of organic solvents, have extraction time short, extract low, the yield advantages of higher of temperature, be a kind of efficient, green, energy-conservation dioscin extracting method.
It should be noted last that: above embodiment is only in order to explanation, and unrestricted technical scheme of the present invention, although the present invention is had been described in detail with reference to the foregoing description, those of ordinary skill in the art is to be understood that: still can make amendment or be equal to replacement the present invention, and not breaking away from any modification or partial replacement of the spirit and scope of the present invention, it all should be encompassed in the middle of the claim scope of the present invention.
Claims (10)
1. the extracting method of a dioscin is characterized in that: may further comprise the steps:
(1) plant drying, the crushing screening that will contain dioscin gets dry powder;
(2) surfactant dissolves is mixed with solvent in water;
(3) solvent that the dry powder and the step (2) of step (1) gained are prepared, the ratio of solvent and dry powder is 0.1: 1～100: 1, extracts with intensified by ultrasonic wave, isolates solid, can obtain containing the extracting solution of dioscin;
(4) extracting solution is handled thick dioscin or thick diosgenin.
2. according to the extracting method of the described a kind of dioscin of claim 1, it is characterized in that: comprise that also thick dioscin from Paris polyphylla Smith is purified or diosgenin is produced in further processing.
3. the extracting method of dioscin according to claim 1 is characterized in that: the tensio-active agent in the described step (2) is any one or its combination in sodium lauryl sulphate, sodium laurylsulfonate, Sodium dodecylbenzene sulfonate, cetyl trimethylammonium bromide, the tween-80.
4. the extracting method of dioscin according to claim 1 is characterized in that: the massfraction of tensio-active agent is 1～50% in the solvent of described step (2) preparation.
5. the extracting method of dioscin according to claim 1 is characterized in that: step (3) applies ultrasonic field and extracts to strengthen when extracting, wherein ultrasonic frequency range is 10～5000KHz.
6. the extracting method of dioscin according to claim 2, it is characterized in that: the treatment process of step (4) extracting solution is: concentrate and add separation concentrated solution after the skim soln degreasing, evaporated under reduced pressure, thick dioscin.
7. the extracting method of dioscin according to claim 6, it is characterized in that: described skim soln is a low-molecular-weight ester, is preferably ethyl acetate, butylacetate, phenylacetate or heptyl acetate.
8. the extracting method of dioscin according to claim 2, it is characterized in that: the treatment process of step (4) extracting solution is: be concentrated into flocks and separate out, collecting precipitation, thick dioscin.
9. the extracting method of dioscin according to claim 2, it is characterized in that: the treatment process of step (4) extracting solution is: directly add an acidic catalyst heating hydrolysis in extracting solution, get thick diosgenin, thick diosgenin can further be purified by the method for recrystallization.
10. the extracting method of dioscin according to claim 9, it is characterized in that: described an acidic catalyst is any one in hydrochloric acid, sulfuric acid or the ion exchange resin.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432665A (en) * | 2011-09-27 | 2012-05-02 | 陕西科技大学 | Alcohol-free extraction method for dioscin |
| CN103880914A (en) * | 2014-03-04 | 2014-06-25 | 陕西科技大学 | Flocculation extraction method of diosgenin |
| CN103965283A (en) * | 2014-04-11 | 2014-08-06 | 陕西科技大学 | Separation method of high-purity diosgenin |
| CN113633566A (en) * | 2021-08-30 | 2021-11-12 | 广州佳成生物科技有限公司 | Preparation method of diosgenin chitosan transfersome |
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2008
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432665A (en) * | 2011-09-27 | 2012-05-02 | 陕西科技大学 | Alcohol-free extraction method for dioscin |
| CN102432665B (en) * | 2011-09-27 | 2013-10-09 | 陕西科技大学 | Alcohol-free extraction method for dioscin |
| CN103880914A (en) * | 2014-03-04 | 2014-06-25 | 陕西科技大学 | Flocculation extraction method of diosgenin |
| CN103880914B (en) * | 2014-03-04 | 2016-05-18 | 陕西科技大学 | A kind of flocculation extracting method of Chinese yam saponin |
| CN103965283A (en) * | 2014-04-11 | 2014-08-06 | 陕西科技大学 | Separation method of high-purity diosgenin |
| CN103965283B (en) * | 2014-04-11 | 2016-02-10 | 陕西科技大学 | A kind of separation method of high purity diosgenin |
| CN113633566A (en) * | 2021-08-30 | 2021-11-12 | 广州佳成生物科技有限公司 | Preparation method of diosgenin chitosan transfersome |
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| CN101591373B (en) | 2012-07-04 |
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