CN102603632B - Method for preparing sinomenine hydrochloride by using non-organic solvent - Google Patents
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Abstract
The invention provides a preparation method of sinomenine hydrochloride. The method comprises the steps of: A) extraction: wetting caulis sinomenii coarse powder by using hydrochloric acid (HCl), installing a percolator, adding HCl for impregnation and percolation to obtain percolate; B) eluting treated cation exchange resin or 152 resin on the percolate by using ammonia water-ethanol solution or HCl with concentration being 3-10 percent, desalting, condensing and drying to obtain sinomenine hydrochloride crude products; and C) taking the sinomenine hydrochloride crude products, heating the crude products in ethanol or purified water for back flowing, condensing filtrate, cooling, crystallizing, filtering and using ethanol to wash a filter cake to obtain the sinomenine hydrochloride. Since the method adopts an absorbing process through the cation exchange resin or large-pore absorbing resin to replace the traditional extraction process through high-toxicity benzene and chloroform, the extraction rate is high, the method is simpler and convenient to operate, the harm and the pollution caused by high quantity of high-toxicity organic solvent to operator health and the environment can be avoided, the treatment process of the organic solvent is reduced, the environmental protection is further facilitated, the investment in environmental protection facilities of a factory is reduced and the environmental-friendly production is facilitated. The sinomenine hydrochloride prepared by adopting the method through extraction and separation can be used as a raw material for pharmaceutical preparations, the purity is higher, solvent residue does not exists and the potential harm to human bodies is reduced.
Description
Technical field
The present invention relates to a kind of preparation method of sinomenine hydrochloride, be specifically related to the method for effective constituent sinomenine hydrochloride in a kind of non-organic solvent extraction Stem of Orientoine.
Background technology
Stem of Orientoine is traditional conventional Chinese medicine, for the dry rattan of menispermaceous plants sinomenium acutum and hair sinomenium acutum, just on the books in Compendium of Material Medica, now record in Pharmacopoeia of the People's Republic of China version in 2010, have dispel the wind, effect of the meridian dredging, diuresis, be used for the treatment of rheumatic arthralgia, arthroncus, paralysis itch, also have the effects such as anti-heart disorder and step-down.
In Stem of Orientoine, main component is alkaloid, the composition of having found at present has tuduranine (Sinomenine), isosinomenine (Igoginomenine), China's tuduranine (SinoAcutine), short sinomenium acutum time alkali (Acutumidine), point tuduranine (Sinaetine) and disinomenine (Diginomenine), ethyl tuduranine (ethylsinomenine), tetrahydrochysene epiberberine (sinactine), tetrahydrochysene epiberberine, yellow parilla ripple phenol alkali, bianfugenine, Tetrahydropalmatine etc.
Tuduranine (Sinomenine) is a kind of alkaloid monomer extracting in Stem of Orientoine, is the main effective constituent of Stem of Orientoine performance analgesia, anti-inflammatory action, is separated and obtains the earliest by Ishiwari etc. from Japanese Stem of Orientoine.The sixties in 20th century, Chinese scholar Zhu Renhong also found tuduranine from domestic Stem of Orientoine.Conventional its hydrochloride preparation, as ZHENGQINGFENGTONGNING PIAN, Zhengqing Fengtongning Retard Tablets, ZHENGQINGFENGTONGNING injection liquid, is used for the treatment of rheumatic, rheumatoid arthritis clinically, and treatment ankylosing spondylitis, irregular pulse etc. are evident in efficacy.
Industrial production sinomenine hydrochloride adopts alkalization water extraction process more at present, and it alkalization for some time, then adds a certain amount of technical benzene, refluxing extraction, last acidifying, standing, crystallization for add water and a certain amount of white lime in Stem of Orientoine.Stem of Orientoine dilute sulphuric acid percolate, adjusts pH value 9 with liming, and benzene carries out counter-current extraction at 50 DEG C, and benzene extraction liquid carries out anti-phase counter-current extraction, activated carbon decolorizing, crystallization with 1% hydrochloric acid.In hot water, carry out recrystallization, obtain sterling.(Chen Yukun " extracting technique of Chinese medicine ", 1992), existing method is all used benzene that toxicity is very large or chloroform as extracting solvent, benzene is one-level noxious solvent, cancer rate processed is very high, disabled at pharmaceutical industry, and need be by very cumbersome technique ability meet the requirement of environmental protection aspect the recycling of solvent, and chloroform is secondary toxic reagent, thereby should avoid using benzene and chloroform solvent in traditional Chinese medicine extraction as far as possible.
Summary of the invention
The invention provides a kind of preparation method of sinomenine hydrochloride of non-organic solvent.
The present invention seeks to be achieved through the following technical solutions:
A preparation method for the sinomenine hydrochloride of non-organic solvent, the method comprises the steps:
A, extraction: Stem of Orientoine meal 100～1000 weight parts, with wetting 0.5～8 hour of 0.1～1mol/L HCl of 60～1000 parts by volume, dress percolator, add again 0.1～1mol/L HCl to make liquid level cover medicinal powder 2cm, flood after 6～48 hours, start diacolation by the speed of 2～5ml/min, after 6～24 hours, stop diacolation, obtain percolate, for subsequent use;
B, upper prop wash-out: by processed good Zeo-karb on percolate or 152 type resins, blade diameter length ratio 1: 8-12, loading speed be 2-5 times of column volume/hour, there is precipitation with the inspection of silicotungstic acid test solution to effluent liquid, and thin-layer chromatography stops loading while detecting lifeless matter alkaline spot point, while being eluted to elutriant without color by purified water, stop, soak resin or 152 type resins 3-10% hydrochloric acid soln with 8-15% ammonia solution and soak resin 12 hours, use again ammoniacal liquor-ethanolic soln wash-out or the 152 type resins 3-10% hydrochloric acid soln wash-out of pH8-11, elution speed is 2-5BV/h, elutriant receives while having precipitation with the inspection of silicotungstic acid test solution, while receiving elutriant silicotungstic acid test solution inspection without precipitation, stop, merge elutriant, with hydrochloric acid or ammonia neutralization to pH=6-8, desalination, concentrate drying, obtain sinomenine hydrochloride crude product.
C, refining: get sinomenine hydrochloride crude product 5～10 weight parts, with 10～95% ethanol or the dissolving extremely completely of purified water reflux of 30～120 parts by volume, add the gac of 3-6% times of weight, insulation refluxes 10～30 minutes, filters while hot, and filtrate is concentrated, cooling, crystallization, filter, clean filter cake with the ethanol of 75-95% colourless to filtrate, obtain sinomenine hydrochloride.
Parameter in the preparation method of sinomenine hydrochloride of the present invention is preferably as follows:
In B step, the preferred 001*2.5 of strong cation-exchanging resin, 001*4, macroporous adsorbent resin is 152 types preferably; Resin blade diameter length ratio preferably 1: 10; Preferably 3 times of column volumes of loading speed/hour; Soak preferably 10% ammonia solution or 5% hydrochloric acid soln of resin; Elute soln using ammoniacal liquor-ethanolic soln of pH8-11 as Zeo-karb, elutriant is neutralized to pH=6～8 with hydrochloric acid; 5%HCl solution is as the elute soln of 152 type macroporous adsorbent resins;
C step, preferably adds the gac of 4% times of weight; When reflux preferably 40%, 55%, 60%, 75%, 80% ethanol.
Weight part in the preparation method of above-mentioned sinomenine hydrochloride and the pass of parts by volume are the relation of g/ml.
The inventive method adopts and replaces by Zeo-karb or absorption with macroporous adsorbent resin benzene extraction and chloroform extraction (extraction) technique that traditional toxicity is larger; extract yield is high; operate easier; the harm and the pollution that overcome that consumption of organic solvent is large, toxicity cause to operator ' s health and environment greatly; reduce the treating processes of organic solvent; more be conducive to environment protection, reduced the input of the environmental protection facility of factory, be conducive to environmental friendliness and produce.Present method is extracted the sinomenine hydrochloride separating, and as the raw material of pharmaceutical preparation, purity is higher, and no solvent residue has reduced the potential hazard to human body.
Following experimental example and embodiment are used for further illustrating but are not limited to the present invention.
Experimental example one: the Study on extraction of Stem of Orientoine non-organic solvent
1, experimental technique
1.1 materials and instrument
Stem of Orientoine medicinal material coarse powder, macroporous adsorbent resin, sinomenine hydrochloride reference substance, hydrochloric acid, ammoniacal liquor, sodium hydroxide, ethanol, sodium-chlor etc.
Glass column (diameter 3cm, high 30～40cm), HPLC high performance liquid phase detector, rotary evaporimeter.
1.2 methods and result
1.2.1 decision method
(1) alkaloid indicator is selected
Press method preparation bismuth potassium iodide dilute solution of Chinese Pharmacopoeia version in 2010, basic iron potassium cyanide, three kinds of alkaloid indicator of silicotungstic acid test solution, getting respectively 1～2 drips in checking liquid, precipitate, color reaction, experiment contrast premenstruum, shows that the instruction of silicotungstic acid test solution is the most directly perceived, sensitive.This experimental design adopts the indicator of silicotungstic acid test solution as endpoint.
(2) thin-layer chromatography: stationary phase: silica gel thin-layer plate; Developping agent: methyl alcohol: water: ammoniacal liquor=8: 1: 1; Developer: rare bismuth potassium iodide solution.
(3) high performance liquid chromatography
With octadecylsilane chemically bonded silica be weighting agent; Taking acetonitrile-0.78% sodium dihydrogen phosphate (12: 88) as moving phase; Detection wavelength is 265nm.30 DEG C of column temperatures, flow velocity 1.0ml/min.
1.2.2. the type selecting of resin
(1) resin model
D-101 type, nonpolar macroporous adsorption resin, manufacturer: Tianjin sea light chemical industry;
LSD001 type, polar macroporous adsorption resin, manufacturer: Xi'an Lanxiao Sci-Tech Co., Ltd.;
D-312 type, macroporous adsorbent resin, manufacturer: Shandong Lukang Record Pharmaceuticals Co., Ltd.;
DM21 type, macroporous adsorbent resin, manufacturer: Shandong Lukang Record Pharmaceuticals Co., Ltd.;
HPD722 type, low-pole macroporous adsorbent resin, manufacturer: Cangzhou Bon Adsorption Material Science and Technology Co., Ltd.
152 types, Zeo-karb, manufacturer: Shandong Lukang Record Pharmaceuticals Co., Ltd.;
732 types, sodium type Zeo-karb, manufacturer: Cangzhou Bon Adsorption Material Science and Technology Co., Ltd.
001 × 2.5 type, H type Zeo-karb, manufacturer: Shandong Lukang Record Pharmaceuticals Co., Ltd.;
001 × 4 type, H type Zeo-karb, manufacturer: Shandong Lukang Record Pharmaceuticals Co., Ltd.;
(2) method
Choose macroporous resin or the ion exchange resin 10g～20g of above-mentioned different manufacturers, different model, upper 30mm*300mm glass exchange column after pre-treatment, get the percolate (pH is adjusted to 3) of 1000g medicinal material, be divided into 7 equal portions, flow through resin by certain speed, general loading speed is 2～3BV/h, the special resin reference velocity of pressing, have to precipitate with the inspection of silicotungstic acid test solution to effluent liquid to stop loading, wash with water to elutriant substantially without till color.Applied sample amount and the adsorptive power of contrast different resins, the resin model of selected good best producer, chooses the sorbing material of 2～3 kinds of resins as this product.
The absorption situation of table 1 different model resin upper prop
Only investigate absorption situation from indicator, thin layer and observe phenomena because of above experiment, cannot accurately judge the absorption situation of resin, the later stage uses liquid chromatography instead associated resin is investigated.
1, sinomenine hydrochloride raw material absorption: the sinomenine hydrochloride solution (2g → 100ml) of preparation 2%, get respectively D101,001*4, tri-kinds of each 2g of resin of DM21 in Erlenmeyer flask, add the above-mentioned obtain solution of 10ml, on repeatedly Turning motion device, shake 12 hours, Liquid Detection, the results are shown in following table
Table 2: the absorption HPLC result of different resins Static Adsorption sinomenine hydrochloride stock liquid
2, extract stoste absorption, get respectively 001*2.5,001*4,152 types, AB-8 type, HPD600 type, 732 types, DM21 type, the treated good resin 2g of D101 type puts in 100ml Erlenmeyer flask, the diacolation stoste 25ml that adds extraction, Liquid Detection, the results are shown in following table:
Table 3: the absorption HPLC result of the percolate that different resins Static Adsorption Stem of Orientoine is extracted
Above result shows, the comparison of above-mentioned several resin absorption ability: 001*2.5 > 001*4 > 152 types.AB-8, HPD600 type, DM21 type, D101 type, 732 types etc. because of adsorptive power in percolate too a little less than.
1.2.3 desorb or wash-out
According to above experimental result, selected 001*2.5,001*4,152 3 kinds of resins.Each resin is tested by following design.
(1) cation-adsorption resin (001*4,001*2.5)
1. 5% ammoniacal liquor liquid.
2. 10% ammoniacal liquor liquid.
3. 95% ethanolic soln.
4. adjust the ethanolic soln of PH to 8-11 with ammoniacal liquor.
5. salt, diluted acid.(the 5%HCl solution of NH4Cl)
6. salt, rare alcohol.(20%NaCl+ ethanolic soln)
Get sour water percolate 500ml, by resin column, be washed till neutrality by purified water with the flow velocity of 2-3BV/h, then the speed wash-out with 2-3BV/h with different elutriants respectively, till lifeless matter alkali reaction.Measure the sinomenine hydrochloride content in each duplicate samples, calculate eluting rate.Contrast elute effect.
The impact of the different elutriants of table 4 on sinomenine hydrochloride elute effect
Above experiment table fruit shows: after resin cation (R.C.) absorption, adopt ammoniacal liquor-ethanolic soln of pH8-11, can obtain good elute effect.
(2) macroporous adsorbent resin (152 type)
1. 50% ethanolic soln.
2. 75% ethanolic soln.
3. 95% ethanolic soln.
4. 5%HCl solution.
Get sour water percolate 500ml, by resin column, be washed till neutrality by purified water with the flow velocity of 2～3BV/h, then the speed wash-out with 2～3BV/h with different elutriants respectively, till lifeless matter alkali reaction.Measure the sinomenine hydrochloride content in each duplicate samples, calculate eluting rate.Contrast elute effect.
Table 5 152 types adopt the impact of different elutriants on sinomenine hydrochloride elute effect
Experimental result shows: adopt different elutriants to carry out desorb to the adsorption liquid of 152 type resins, only HCl has desorption effect, therefore this resin adopts 5%HCl to carry out wash-out.
1.2.3 Static Adsorption is determined desorption condition
By the selected good elutriant of above-mentioned experiment, adopt the mode of Static Adsorption, after absorption 12 hours, by resin with purified water rinsing in water when lifeless matter alkali, add 12ml stripping liquid, shake Liquid Detection 12 hours.Result is as follows:
The percolate adsorption and desorption HPLC result that table 6 Static Adsorption Stem of Orientoine is extracted
Above result shows, adopts definite stripping liquid to carry out desorb, all can separate the sinomenine hydrochloride of sucking-off resin absorption.
1.3 conclusion
Adopt macroporous adsorbent resin and Zeo-karb, sinomenine hydrochloride is had to larger adsorption, by experiment, selected 001*2.5, bis-kinds of Zeo-karbs of 001*4,152 type macroporous adsorbent resins are as the optimum resin of this sinomenine hydrochloride purification, adopt the elute soln of ammoniacal liquor-ethanolic soln (pH8～11) as Zeo-karb, 5%HCl is as the elute soln of 152 type macroporous adsorbent resins.
Following embodiment all can realize the effect of above-mentioned experimental example.
Embodiment mono-: a kind of preparation method of sinomenine hydrochloride of non-organic solvent, the method comprises the steps:
A, extraction: Stem of Orientoine meal 500kg, uses the 0.5mol/L HCl of 500L to soak 3 hours, dress percolator, add again 0.5mol/L HCl to make liquid level cover medicinal powder 2cm, flood after 12 hours, start diacolation by the speed of 3ml/min, after 12 hours, stop diacolation, obtain percolate, for subsequent use;
B, upper prop wash-out: by processed good Zeo-karb on percolate or 152 type resins, blade diameter length ratio 1: 10, loading speed be 3 times of column volumes/hour, there is precipitation with the inspection of silicotungstic acid test solution to effluent liquid, and thin-layer chromatography stops loading while detecting lifeless matter alkaline spot point, while being eluted to elutriant without color by purified water, stop, with 5% hydrochloric acid soln immersion resin 12h for 10% ammonia solution immersion resin or 152 type resins, adjust the ethanolic soln wash-out of PH to 9 or 5% hydrochloric acid soln wash-out for 152 type resins with 10% ammoniacal liquor again, elution speed is 3BV/h, elutriant receives while having precipitation with the inspection of silicotungstic acid test solution, while receiving elutriant silicotungstic acid test solution inspection without precipitation, stop, merge elutriant, with hydrochloric acid or with ammonia neutralization to pH=6～8, desalination, concentrate drying, obtain sinomenine hydrochloride crude product.
C, refining: get sinomenine hydrochloride crude product 8kg, with 75% ethanol or the dissolving extremely completely of purified water reflux of 100L, add 5% bulking value gac doubly, insulation refluxes 20 minutes, filters while hot, and filtrate is concentrated, cooling, crystallization, filter, it is colourless to filtrate that the ethanol with 80% cleans filter cake, obtains sinomenine hydrochloride.
Embodiment bis-: a kind of preparation method of sinomenine hydrochloride of non-organic solvent, the method comprises the steps:
A, extraction: Stem of Orientoine meal 800kg, uses the 0.9mol/L HCl of 1000L to soak 5 hours, dress percolator, add again 0.9mol/L HCl to make liquid level cover medicinal powder 2cm, flood after 20 hours, start diacolation by the speed of 5ml/min, after 24 hours, stop diacolation, obtain percolate, for subsequent use;
B, upper prop wash-out: by processed good Zeo-karb 001*4 type or 152 type resins on percolate, blade diameter length ratio 1: 10, loading speed be 5 times of column volumes/hour, there is precipitation with the inspection of silicotungstic acid test solution to effluent liquid, and thin-layer chromatography stops loading while detecting lifeless matter alkaline spot point, while being eluted to elutriant without color by purified water, stop, soak resin or 152 type resins 8% hydrochloric acid soln immersion resin 12 hours with 10% ammonia solution, adjust again ethanolic soln wash-out or the 152 type resin 8% hydrochloric acid soln wash-outs of PH to 9 with 12% ammoniacal liquor, elution speed is 5BV/h, elutriant receives while having precipitation with the inspection of silicotungstic acid test solution, while receiving elutriant silicotungstic acid test solution inspection without precipitation, stop, merge elutriant, with hydrochloric acid neutralization or with ammonia neutralization to pH=7, desalination, concentrate drying, obtain sinomenine hydrochloride crude product.
C, refining: get sinomenine hydrochloride crude product 10kg, with 85% ethanol or the dissolving extremely completely of purified water reflux of 120L, add 5% bulking value gac doubly, insulation refluxes 30 minutes, filters while hot, and filtrate is concentrated, cooling, crystallization, filter, it is colourless to filtrate that the ethanol with 75% cleans filter cake, obtains sinomenine hydrochloride.
Embodiment tri-: a kind of preparation method of sinomenine hydrochloride of non-organic solvent, the method comprises the steps:
A, extraction: Stem of Orientoine meal 800kg, uses the 0.7mol/L HCl of 900L to soak 6 hours, dress percolator, add again 0.8mol/L HCl to make liquid level cover medicinal powder 2cm, flood after 24 hours, start diacolation by the speed of 3ml/min, after 24 hours, stop diacolation, obtain percolate, for subsequent use;
B, upper prop wash-out: by processed good Zeo-karb on percolate or 152 type resins, blade diameter length ratio 1: 10, loading speed is 3 times of column volume/h, there is precipitation with the inspection of silicotungstic acid test solution to effluent liquid, and thin-layer chromatography stops loading while detecting lifeless matter alkaline spot point, while being eluted to elutriant without color by purified water, stop, soak resin or 152 type resins 7% hydrochloric acid soln immersion resin 12 hours with 10% ammonia solution, adjust again ethanolic soln wash-out or the 152 type resin 5% hydrochloric acid soln wash-outs of PH to 9 with 12% ammoniacal liquor, elution speed is 4BV/h, elutriant receives while having precipitation with the inspection of silicotungstic acid test solution, while receiving elutriant silicotungstic acid test solution inspection without precipitation, stop, merge elutriant, with hydrochloric acid or with ammonia neutralization to pH=7, desalination, concentrate drying, obtain sinomenine hydrochloride crude product.
C, refining: get sinomenine hydrochloride crude product 6kg, with 55% ethanol or the dissolving extremely completely of purified water reflux of 80L, add 3% bulking value gac doubly, insulation refluxes 10～30 minutes, filters while hot, and filtrate is concentrated, cooling, crystallization, filter, it is colourless to filtrate that the ethanol with 80% cleans filter cake, obtains sinomenine hydrochloride.
Attached: 1, silicotungstic acid test solution inspection method
Silicotungstic acid test solution preparation: press annex 109 of Chinese Pharmacopoeia version in 2010.
Get 1ml and be examined liquid in colorimetric cylinder, add 1 to 2 silicotungstic acid test solution, observe.
2, thin layer chromatography
Thin-layer chromatography condition stationary phase: silica gel thin-layer plate
Developping agent: methyl alcohol: water: ammoniacal liquor=8: 1: 1
Developer: bismuth potassium iodide dilute solution
Point sample amount: 5ul
3, ammoniacal liquor-ethanolic soln of pH8-11 adjusts the ethanolic soln of pH to 8～11 with the ammoniacal liquor of 8-15%.
Claims (4)
1. non-organic solvent is prepared a method for sinomenine hydrochloride, it is characterized in that the method comprises the steps:
A, extraction: Stem of Orientoine meal 100～1000 weight parts, with wetting 0.5～8 hour of 0.1～1mol/L HCl of 60～1000 parts by volume, dress percolator, add again 0.1～1mol/L HCl to make liquid level cover medicinal powder 2cm, flood after 6～48 hours, start diacolation by the speed of 2～5ml/min, after 6～24 hours, stop diacolation, obtain percolate, for subsequent use;
B, upper prop wash-out: by processed good Zeo-karb on percolate, blade diameter length ratio 1: 8-12, loading speed be 2-5 times of column volume/hour, there is precipitation with the inspection of silicotungstic acid test solution to effluent liquid, and thin-layer chromatography stops loading while detecting lifeless matter alkaline spot point, while being eluted to elutriant without color by purified water, stop, soak Zeo-karb 12 hours with 8-15% ammonia solution, use again ammoniacal liquor-ethanolic soln wash-out of pH8-11, elution speed be 2-5 times of column volume/hour, elutriant receives while having precipitation with the inspection of silicotungstic acid test solution, while receiving elutriant silicotungstic acid test solution inspection without precipitation, stop, merge elutriant, be neutralized to pH=6-8 with hydrochloric acid, desalination, concentrate drying, obtain sinomenine hydrochloride crude product, described Zeo-karb is 001 × 2.5 type H type Zeo-karb, 001 × 4 type H type Zeo-karb,
C, refining: get sinomenine hydrochloride crude product 5～10 weight parts, with 10～95% ethanol or the dissolving extremely completely of purified water reflux of 30～120 parts by volume, add 3-6% bulking value gac doubly, insulation refluxes 10～30 minutes, filters while hot, and filtrate is concentrated, cooling, crystallization, filter, clean filter cake with the ethanol of 75-95% colourless to filtrate, obtain sinomenine hydrochloride;
Weight part in the preparation method of described sinomenine hydrochloride and the pass of parts by volume are the relation of g/ml.
2. the method for preparing sinomenine hydrochloride as claimed in claim 1, is characterized in that, in the method B step, resin blade diameter length ratio is 1: 10; Loading speed be 3 times of column volumes/hour.
3. the method for preparing sinomenine hydrochloride as claimed in claim 1 or 2, is characterized in that in the method B step, soaks Zeo-karb 10% ammonia solution; Elute soln using ammoniacal liquor-ethanolic soln of pH8-11 as Zeo-karb.
4. the method for preparing sinomenine hydrochloride as claimed in claim 1 or 2, is characterized in that in the method C step, adds 4% bulking value gac doubly; When reflux, alcohol concn is 40%, 55%, 60%, 75% or 80%.
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| CN106236700A (en) * | 2016-08-04 | 2016-12-21 | 长沙原道医药科技开发有限公司 | Sinomenine hydrochloride ointment prepared by a kind of organic solvent and preparation method thereof |
| CN106137949A (en) * | 2016-08-04 | 2016-11-23 | 长沙原道医药科技开发有限公司 | Sinomenine hydrochloride ointment prepared by a kind of inorganic solvent and preparation method thereof |
| CN106265516A (en) * | 2016-08-04 | 2017-01-04 | 长沙原道医药科技开发有限公司 | Sinomenine hydrochloride spray prepared by a kind of inorganic solvent and preparation method thereof |
| CN106176577A (en) * | 2016-08-04 | 2016-12-07 | 长沙原道医药科技开发有限公司 | Sinomenine hydrochloride gel prepared by a kind of inorganic solvent and preparation method thereof |
| CN106176578A (en) * | 2016-08-04 | 2016-12-07 | 长沙原道医药科技开发有限公司 | Sinomenine hydrochloride gel prepared by a kind of organic solvent and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1125724A (en) * | 1995-11-15 | 1996-07-03 | 西安天诚医药生物工程有限公司 | Preparation method of diversine |
| CN1405167A (en) * | 2002-07-05 | 2003-03-26 | 上海中医药大学 | Method for purifying diversine |
-
2012
- 2012-03-26 CN CN201210081909.5A patent/CN102603632B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1125724A (en) * | 1995-11-15 | 1996-07-03 | 西安天诚医药生物工程有限公司 | Preparation method of diversine |
| CN1405167A (en) * | 2002-07-05 | 2003-03-26 | 上海中医药大学 | Method for purifying diversine |
Non-Patent Citations (2)
| Title |
|---|
| 张晓伟.青藤碱提取工艺的优化.《中医药信息》.2002,第19卷(第5期),第55页. |
| 青藤碱提取工艺的优化;张晓伟;《中医药信息》;20021231;第19卷(第5期);第55页 * |
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