CN104072572A - Glycyrrhetinic acid sodium and preparation method thereof - Google Patents
Glycyrrhetinic acid sodium and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- MPDGHEJMBKOTSU-YKLVYJNSSA-N 18beta-glycyrrhetic acid Chemical compound C([C@H]1C2=CC(=O)[C@H]34)[C@@](C)(C(O)=O)CC[C@]1(C)CC[C@@]2(C)[C@]4(C)CC[C@@H]1[C@]3(C)CC[C@H](O)C1(C)C MPDGHEJMBKOTSU-YKLVYJNSSA-N 0.000 title abstract description 22
- 229960003720 enoxolone Drugs 0.000 title abstract description 12
- MPDGHEJMBKOTSU-UHFFFAOYSA-N Glycyrrhetinsaeure Natural products C12C(=O)C=C3C4CC(C)(C(O)=O)CCC4(C)CCC3(C)C1(C)CCC1C2(C)CCC(O)C1(C)C MPDGHEJMBKOTSU-UHFFFAOYSA-N 0.000 title abstract description 11
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 title abstract 5
- 229910052708 sodium Inorganic materials 0.000 title abstract 5
- 239000011734 sodium Substances 0.000 title abstract 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 52
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 45
- LPLVUJXQOOQHMX-QWBHMCJMSA-N glycyrrhizinic acid Chemical compound O([C@@H]1[C@@H](O)[C@H](O)[C@H](O[C@@H]1O[C@@H]1C([C@H]2[C@]([C@@H]3[C@@]([C@@]4(CC[C@@]5(C)CC[C@@](C)(C[C@H]5C4=CC3=O)C(O)=O)C)(C)CC2)(C)CC1)(C)C)C(O)=O)[C@@H]1O[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@H]1O LPLVUJXQOOQHMX-QWBHMCJMSA-N 0.000 claims abstract description 18
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- MOCOXAJEZKHXSF-IHMBCTQLSA-M sodium;(2s,4as,6ar,6as,6br,8ar,10s,12as,14br)-10-hydroxy-2,4a,6a,6b,9,9,12a-heptamethyl-13-oxo-3,4,5,6,6a,7,8,8a,10,11,12,14b-dodecahydro-1h-picene-2-carboxylate Chemical compound [Na+].C([C@H]1C2=CC(=O)[C@H]34)[C@@](C)(C([O-])=O)CC[C@]1(C)CC[C@@]2(C)[C@]4(C)CC[C@@H]1[C@]3(C)CC[C@H](O)C1(C)C MOCOXAJEZKHXSF-IHMBCTQLSA-M 0.000 claims description 26
- 229960004756 ethanol Drugs 0.000 claims description 15
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 238000010992 reflux Methods 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 7
- OVYTZAASVAZITK-UHFFFAOYSA-M sodium;ethanol;hydroxide Chemical compound [OH-].[Na+].CCO OVYTZAASVAZITK-UHFFFAOYSA-M 0.000 claims description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 230000015572 biosynthetic process Effects 0.000 claims description 6
- 238000002425 crystallisation Methods 0.000 claims description 6
- 230000003750 conditioning effect Effects 0.000 claims description 5
- 230000008025 crystallization Effects 0.000 claims description 5
- 238000004821 distillation Methods 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 2
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 2
- 239000000047 product Substances 0.000 abstract description 5
- 230000003110 anti-inflammatory effect Effects 0.000 abstract description 3
- 239000002904 solvent Substances 0.000 abstract description 3
- 229960004949 glycyrrhizic acid Drugs 0.000 abstract description 2
- 235000019410 glycyrrhizin Nutrition 0.000 abstract description 2
- 238000007086 side reaction Methods 0.000 abstract description 2
- 239000002244 precipitate Substances 0.000 abstract 6
- 235000019441 ethanol Nutrition 0.000 abstract 3
- 238000010438 heat treatment Methods 0.000 abstract 2
- 239000000243 solution Substances 0.000 abstract 2
- VTAJIXDZFCRWBR-UHFFFAOYSA-N Licoricesaponin B2 Natural products C1C(C2C(C3(CCC4(C)CCC(C)(CC4C3=CC2)C(O)=O)C)(C)CC2)(C)C2C(C)(C)CC1OC1OC(C(O)=O)C(O)C(O)C1OC1OC(C(O)=O)C(O)C(O)C1O VTAJIXDZFCRWBR-UHFFFAOYSA-N 0.000 abstract 1
- 239000007864 aqueous solution Substances 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- LPLVUJXQOOQHMX-UHFFFAOYSA-N glycyrrhetinic acid glycoside Natural products C1CC(C2C(C3(CCC4(C)CCC(C)(CC4C3=CC2=O)C(O)=O)C)(C)CC2)(C)C2C(C)(C)C1OC1OC(C(O)=O)C(O)C(O)C1OC1OC(C(O)=O)C(O)C(O)C1O LPLVUJXQOOQHMX-UHFFFAOYSA-N 0.000 abstract 1
- UYRUBYNTXSDKQT-UHFFFAOYSA-N glycyrrhizic acid Natural products CC1(C)C(CCC2(C)C1CCC3(C)C2C(=O)C=C4C5CC(C)(CCC5(C)CCC34C)C(=O)O)OC6OC(C(O)C(O)C6OC7OC(O)C(O)C(O)C7C(=O)O)C(=O)O UYRUBYNTXSDKQT-UHFFFAOYSA-N 0.000 abstract 1
- 239000001685 glycyrrhizic acid Substances 0.000 abstract 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 231100000614 poison Toxicity 0.000 abstract 1
- 230000007096 poisonous effect Effects 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 239000012467 final product Substances 0.000 description 9
- 239000007791 liquid phase Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 4
- -1 Glycyrrhizinic acid monopotassium salt Chemical class 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 2
- 150000002342 glycyrrhetinic acids Chemical class 0.000 description 2
- NOESYZHRGYRDHS-UHFFFAOYSA-N insulin Chemical compound N1C(=O)C(NC(=O)C(CCC(N)=O)NC(=O)C(CCC(O)=O)NC(=O)C(C(C)C)NC(=O)C(NC(=O)CN)C(C)CC)CSSCC(C(NC(CO)C(=O)NC(CC(C)C)C(=O)NC(CC=2C=CC(O)=CC=2)C(=O)NC(CCC(N)=O)C(=O)NC(CC(C)C)C(=O)NC(CCC(O)=O)C(=O)NC(CC(N)=O)C(=O)NC(CC=2C=CC(O)=CC=2)C(=O)NC(CSSCC(NC(=O)C(C(C)C)NC(=O)C(CC(C)C)NC(=O)C(CC=2C=CC(O)=CC=2)NC(=O)C(CC(C)C)NC(=O)C(C)NC(=O)C(CCC(O)=O)NC(=O)C(C(C)C)NC(=O)C(CC(C)C)NC(=O)C(CC=2NC=NC=2)NC(=O)C(CO)NC(=O)CNC2=O)C(=O)NCC(=O)NC(CCC(O)=O)C(=O)NC(CCCNC(N)=N)C(=O)NCC(=O)NC(CC=3C=CC=CC=3)C(=O)NC(CC=3C=CC=CC=3)C(=O)NC(CC=3C=CC(O)=CC=3)C(=O)NC(C(C)O)C(=O)N3C(CCC3)C(=O)NC(CCCCN)C(=O)NC(C)C(O)=O)C(=O)NC(CC(N)=O)C(O)=O)=O)NC(=O)C(C(C)CC)NC(=O)C(CO)NC(=O)C(C(C)O)NC(=O)C1CSSCC2NC(=O)C(CC(C)C)NC(=O)C(NC(=O)C(CCC(N)=O)NC(=O)C(CC(N)=O)NC(=O)C(NC(=O)C(N)CC=1C=CC=CC=1)C(C)C)CC1=CN=CN1 NOESYZHRGYRDHS-UHFFFAOYSA-N 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 230000000144 pharmacologic effect Effects 0.000 description 2
- TWCMVXMQHSVIOJ-UHFFFAOYSA-N Aglycone of yadanzioside D Natural products COC(=O)C12OCC34C(CC5C(=CC(O)C(O)C5(C)C3C(O)C1O)C)OC(=O)C(OC(=O)C)C24 TWCMVXMQHSVIOJ-UHFFFAOYSA-N 0.000 description 1
- PLMKQQMDOMTZGG-UHFFFAOYSA-N Astrantiagenin E-methylester Natural products CC12CCC(O)C(C)(CO)C1CCC1(C)C2CC=C2C3CC(C)(C)CCC3(C(=O)OC)CCC21C PLMKQQMDOMTZGG-UHFFFAOYSA-N 0.000 description 1
- 102000004877 Insulin Human genes 0.000 description 1
- 108090001061 Insulin Proteins 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical class [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000005903 acid hydrolysis reaction Methods 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 230000001741 anti-phlogistic effect Effects 0.000 description 1
- 230000000840 anti-viral effect Effects 0.000 description 1
- 239000003699 antiulcer agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000004700 cellular uptake Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- OCLXJTCGWSSVOE-UHFFFAOYSA-N ethanol etoh Chemical compound CCO.CCO OCLXJTCGWSSVOE-UHFFFAOYSA-N 0.000 description 1
- PFOARMALXZGCHY-UHFFFAOYSA-N homoegonol Natural products C1=C(OC)C(OC)=CC=C1C1=CC2=CC(CCCO)=CC(OC)=C2O1 PFOARMALXZGCHY-UHFFFAOYSA-N 0.000 description 1
- 229940125396 insulin Drugs 0.000 description 1
- 235000021374 legumes Nutrition 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000001473 noxious effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- WNIFXKPDILJURQ-UHFFFAOYSA-N stearyl glycyrrhizinate Natural products C1CC(O)C(C)(C)C2CCC3(C)C4(C)CCC5(C)CCC(C(=O)OCCCCCCCCCCCCCCCCCC)(C)CC5C4=CC(=O)C3C21C WNIFXKPDILJURQ-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Landscapes
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses glycyrrhetinic acid sodium and a preparation method thereof. The preparation method comprises the following steps: (1) adding a sulfuric acid alcohol solution into glycyrrhizic acid powder; then, carrying out reflux-heating, filtrating and drying to acquire a precipitate a; (2) adding the precipitate a into a sodium hydroxide aqueous solution, and carrying out reflux-heating, cooling, adjusting the solution pH value to 2 to 3, filtrating, and washing to acquire a precipitate b; (3) adding ethyl alcohol into the precipitate b to dissolve the precipitate b; then, adding sodium hydroxide ethyl alcohol into the precipitate b; carrying out stirring, vacuum distilling, drying and smashing to acquire the glycyrrhetinic acid sodium. According to the preparation method of the glycyrrhetinic acid sodium, a poisonous solvent is not adopted, so that the side reaction is less, and the preparation method is safe and environmental-friendly; besides, the glycyrrhetinic acid sodium product prepared by the preparation method is high in yield, low in cost, and obvious in anti-inflammatory effect; moreover, the preparation method is further good in practicability, and can be suitable for industrial large-scale production.
Description
Technical field
The present invention relates to a kind of Sodium glycyrrhetinate and preparation method thereof, belong to Chemicals synthesis technical field.
Background technology
Glycyrrhizic legume is medicinal material conventional in Chinese medicine.Research shows that its main pharmacological active substance is Potenlini and aglycone glycyrrhetinic acid thereof.The pharmacological action of Potenlini is actually the effectiveness of glycyrrhetinic acid, glycyrrhetinic acid has anti-inflammatory, antiulcer agent, antiviral, reducing blood-fat, anti-curing oncoma, promotes many-sided effect [Jin Hui such as absorption of insulin, Mao Shengjun, Zhang Kun, et al., the research [J] of the synthetic and Isolated Rat Liver cellular uptake of glycyrrhetinic acid analog derivative. West China pharmaceutical journal, 2010,25 (6): 652-654.].
Nineteen thirty-seven W.Voss and P.Klcin be synthetic first Enoxolone derivative---glycyrrhetinic acid mono-ammonium and monopotassium salt first, and this salt derivative has stronger anti-inflammatory, and the less [W.Voss of untoward reaction; .Klcin.BerTOB.1937:122-132CFAngewChem, 1936; 49:556], but be correlated with and report with it there are no the production technique of Sodium glycyrrhetinate.
Prepared the preparation method of Enoxolone derivative, be generally taking Glycyrrhizinic acid monopotassium salt or ammonium salt as raw material in the past, through adding sulphuric acid hydrolysis, filters, and the glycyrrhetinic acid purity obtaining is like this very poor, and be difficult to purification with common crystallization method.Moreover the general chloroform that adopts as solvent more, in the patent that is called " C30H45O4K and production technique thereof and purposes " that is 00137741.8 at application number, adopt chloroform toxicity larger, and be not suitable for suitability for industrialized production, turnout is also restricted, and the Enoxolone derivative preparing with the low glycyrrhetinic acid of purity is subject to purity and production quantitative limitation equally.
Summary of the invention
In order to overcome prior art problem, the object of the present invention is to provide that a kind of purity is high, the preparation method of the Sodium glycyrrhetinate that is easy to suitability for industrialized production.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
A kind of Sodium glycyrrhetinate, is characterized in that, molecular formula is C30H45O4Na, and molecular weight is 492, and structural formula is shown in formula (Ι):
（Ι）。
A preparation method for Sodium glycyrrhetinate, is characterized in that, comprises the following steps:
(1) prepare throw out a: will in Potenlini powder, add alcohol sulfate solution, described alcohol sulfate solution and the mass ratio of Potenlini powder are (2 ~ 6): 1, if preferred mass is more very few than the amount that is 4:1(alcohol, solution viscosity is large, Potenlini sticky on reactor wall is easily baked and is stuck with paste, and affects yield, and as excessive in the amount of alcohol, the acid using is more, uneconomical), then, reflux 6 ~ 8h under the temperature condition of 90 ~ 110 DEG C, be cooled to crystallization, after filtering and drying, be precipitated thing a at 50 ~ 65 DEG C; ;
(2) prepare throw out b: the throw out a that step (1) is prepared joins in aqueous sodium hydroxide solution, the quality that adds of described aqueous sodium hydroxide solution is 2 ~ 5 times of throw out a quality, preferably 3 times, then, under the temperature condition of 80 ~ 90 DEG C, reflux to solution is clarified, and is then cooled to normal temperature, with the pH value of hydrochloric acid conditioning solution be 2 ~ 3, by the precipitation of formation after filtration, wash with water 1 ~ 2 time, at 50 ~ 65 DEG C dry after be precipitated thing b;
(3) prepare Sodium glycyrrhetinate: in the throw out b preparing to step (2), add ethanol, the quality that adds of ethanol is 2 ~ 5 times of throw out b quality, preferably 3 times, after throw out b is dissolved, add the equimolar sodium hydroxide ethanol with throw out b, after stirring, temperature be 55 DEG C, pressure be-condition of 0.1MPa under underpressure distillation, reclaim ethanol, then drying, grind, cross 100 mesh sieves, obtain Sodium glycyrrhetinate.
Further, in the Potenlini powder described in step (1), the content of Potenlini is 65 ~ 85%.
In alcohol sulfate solution described in step (1), the quality percentage composition of sulfuric acid is 15 ~ 20%, preferably 18%.
Alcohol in described alcohol sulfate solution is any in methyl alcohol, ethanol, Virahol, propyl carbinol.
In aqueous sodium hydroxide solution described in step (2), the quality percentage composition of sodium hydroxide is 10 ~ 20%.
Ethanol ethanol described in step (3) is dehydrated alcohol.
And the concentration of sodium hydroxide is 20% ~ 40% in the sodium hydroxide ethanol described in step (3).
Beneficial effect of the present invention is: in the preparation method of Sodium glycyrrhetinate of the present invention, do not adopt noxious solvent, side reaction is few, safety and environmental protection, and its Sodium glycyrrhetinate product yield of preparing is high, and cost is low, antiphlogistic effects is obvious, in addition, described preparation method also has practical, is applicable to the advantage that large-scale industrialization is produced.
Brief description of the drawings
Fig. 1 is the high-efficient liquid phase chromatogram of the final product for preparing of embodiment 1;
Fig. 2 is the high-efficient liquid phase chromatogram of the final product for preparing of embodiment 2;
Fig. 3 is the high-efficient liquid phase chromatogram of the final product for preparing of embodiment 3.
Embodiment
Describe the present invention in detail below in conjunction with specific embodiment.
embodiment 1:
(1) prepare throw out a: will in Potenlini powder (content of Potenlini is 85%) 5kg, add the alcohol sulfate solution that 20kg sulfuric acid quality percentage composition is 18%, then, reflux 8h under the temperature condition of 100 DEG C, be cooled to crystallization, filter and dry at 60 DEG C, obtain 2.21kg throw out a;
(2) prepare throw out b: the 2.21kg throw out a that step (1) is prepared joins in the aqueous sodium hydroxide solution that 6.27kg quality percentage composition is 15%, then, under the temperature condition of 85 DEG C, reflux to solution is clarified, then be cooled to normal temperature, with the pH value of hydrochloric acid conditioning solution be 2 ~ 3, by the precipitation of formation after filtration, wash with water 1 ~ 2 time, at 60 DEG C dry after obtain 1.98kg throw out b;
(3) prepare Sodium glycyrrhetinate: in the 1.98kg throw out b preparing to step (2), add 25L ethanol, after throw out b is dissolved, add 0.17kg sodium hydroxide ethanol, after stirring, ethanol is reclaimed in underpressure distillation (0.1MPa, 55 DEG C), and residue is dried, ground, cross 100 mesh sieves, obtain 2.08kg product.
Fig. 1 is the high-efficient liquid phase chromatogram of the final product for preparing of embodiment 1.
As shown in Figure 1: the content > 90% of Sodium glycyrrhetinate in final product.
Embodiment 2:
(1) prepare throw out a: will in Potenlini powder (content of Potenlini is 75%) 5kg, add the alcohol sulfate solution that 20kg sulfuric acid quality percentage composition is 18%, then, reflux 7h under the temperature condition of 100 DEG C, be cooled to crystallization, filter and dry at 60 DEG C, obtain 2.02kg throw out a;
(2) prepare throw out b: the 2.02kg throw out a that step (1) is prepared joins in the aqueous sodium hydroxide solution that 6.27kg quality percentage composition is 15%, then, under the temperature condition of 85 DEG C, reflux to solution is clarified, then be cooled to normal temperature, with the pH value of hydrochloric acid conditioning solution be 2 ~ 3, by the precipitation of formation after filtration, wash with water 1 ~ 2 time, at 60 DEG C dry after obtain 1.85kg throw out b;
(3) prepare Sodium glycyrrhetinate: in the 1.85kg throw out b preparing to step (2), add 25L ethanol, after throw out b is dissolved, add 0.17kg sodium hydroxide ethanol, after stirring, ethanol is reclaimed in underpressure distillation (0.1MPa, 55 DEG C), and residue is dried, ground, cross 100 mesh sieves, obtain 1.95kg product.
Fig. 2 is the high-efficient liquid phase chromatogram of the final product for preparing of embodiment 2.
As shown in Figure 2: the content > 90% of Sodium glycyrrhetinate in final product.
Embodiment 3:
(1) prepare throw out a: will in Potenlini powder (content of Potenlini is 65%) 5kg, add the alcohol sulfate solution that 20kg sulfuric acid quality percentage composition is 18%, then, reflux 6h under the temperature condition of 100 DEG C, be cooled to crystallization, filter and dry at 60 DEG C, obtain 1.98kg throw out a;
(2) prepare throw out b: the 1.98kg throw out a that step (1) is prepared joins in the aqueous sodium hydroxide solution that 6.27kg quality percentage composition is 15%, then, under the temperature condition of 85 DEG C, reflux to solution is clarified, then be cooled to normal temperature, with the pH value of hydrochloric acid conditioning solution be 2 ~ 3, by the precipitation of formation after filtration, wash with water 1 ~ 2 time, at 60 DEG C dry after obtain 1.81kg throw out b;
(3) prepare Sodium glycyrrhetinate: in the 1.81kg throw out b preparing to step (2), add 25L ethanol, after throw out b is dissolved, add 0.17kg sodium hydroxide ethanol, after stirring, ethanol is reclaimed in underpressure distillation (0.1MPa, 55 DEG C), and residue is dried, ground, cross 100 mesh sieves, obtain 1.88kg product.
Fig. 3 is the high-efficient liquid phase chromatogram of the final product for preparing of embodiment 3.
As shown in Figure 3: the content > 85% of Sodium glycyrrhetinate in final product.
The present invention is illustrated and should be appreciated that above-described embodiment does not limit the present invention in any form according to above-described embodiment, and all employings are equal to replaces or the technical scheme that obtains of equivalent transformation mode, within all dropping on protection scope of the present invention.
Claims (8)
1. a Sodium glycyrrhetinate, is characterized in that, molecular formula is C30H45O4Na, and molecular weight is 492, and structural formula is shown in formula (Ι):
（Ι）。
2. a preparation method for Sodium glycyrrhetinate, is characterized in that, comprises the following steps:
(1) prepare throw out a: alcohol sulfate solution will be added in Potenlini powder, described alcohol sulfate solution and the mass ratio of Potenlini powder are (2 ~ 6): 1, then, reflux 6 ~ 8h under the temperature condition of 90 ~ 110 DEG C, be cooled to crystallization, after filtering and drying, be precipitated thing a at 50 ~ 65 DEG C;
(2) prepare throw out b: the throw out a that step (1) is prepared joins in aqueous sodium hydroxide solution, the quality that adds of described aqueous sodium hydroxide solution is 2 ~ 5 times of throw out a quality, then, under the temperature condition of 80 ~ 90 DEG C, reflux to solution is clarified, then be cooled to normal temperature, with the pH value of hydrochloric acid conditioning solution be 2 ~ 3, by the precipitation of formation after filtration, wash with water 1 ~ 2 time, at 50 ~ 60 DEG C dry after be precipitated thing b;
(3) prepare Sodium glycyrrhetinate: in the throw out b preparing to step (2), add ethanol, the quality that adds of ethanol is 2 ~ 5 times of throw out b quality, after throw out b is dissolved, add the equimolar sodium hydroxide ethanol with throw out b, after stirring, temperature be 55 DEG C, pressure be-condition of 0.1MPa under underpressure distillation, reclaim ethanol, again drying, grind, cross 100 mesh sieves, obtain Sodium glycyrrhetinate.
3. the preparation method of a kind of Sodium glycyrrhetinate according to claim 2, is characterized in that, in the Potenlini powder described in step (1), the content of Potenlini is 65 ~ 85%.
4. the preparation method of a kind of Sodium glycyrrhetinate according to claim 2, is characterized in that, in the alcohol sulfate solution described in step (1), the quality percentage composition of sulfuric acid is 15 ~ 20%.
5. the preparation method of a kind of Sodium glycyrrhetinate according to claim 2, is characterized in that, the alcohol in the alcohol sulfate solution described in step (1) is any in methyl alcohol, ethanol, Virahol, propyl carbinol.
6. the preparation method of a kind of Sodium glycyrrhetinate according to claim 2, is characterized in that, in the aqueous sodium hydroxide solution described in step (2), the quality percentage composition of sodium hydroxide is 10 ~ 20%.
7. the preparation method of a kind of Sodium glycyrrhetinate according to claim 2, is characterized in that, the ethanol described in step (3) is dehydrated alcohol.
8. the preparation method of a kind of Sodium glycyrrhetinate according to claim 2, is characterized in that, in the sodium hydroxide ethanol described in step (3), the concentration of sodium hydroxide is 20% ~ 40%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410346545.8A CN104072572B (en) | 2014-07-21 | 2014-07-21 | A kind of Monosodium glycyrrhetin and preparation method thereof |
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| CN102276678A (en) * | 2011-06-02 | 2011-12-14 | 甘肃亚兰药业有限公司 | Method for preparing glycyrrhetinic acid |
| CN102614213A (en) * | 2012-02-23 | 2012-08-01 | 武汉华纳联合药业有限公司 | Application of glycyrrhizic acid, glycyrrhetinic acid or salt thereof as well as gel composition and preparation method for gel composition |
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