CN104311489A - Green environmentally-friendly industrial sinomenine extraction and separation method - Google Patents
Green environmentally-friendly industrial sinomenine extraction and separation method Download PDFInfo
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- CN104311489A CN104311489A CN201410462640.4A CN201410462640A CN104311489A CN 104311489 A CN104311489 A CN 104311489A CN 201410462640 A CN201410462640 A CN 201410462640A CN 104311489 A CN104311489 A CN 104311489A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D221/00—Heterocyclic compounds containing six-membered rings having one nitrogen atom as the only ring hetero atom, not provided for by groups C07D211/00 - C07D219/00
- C07D221/02—Heterocyclic compounds containing six-membered rings having one nitrogen atom as the only ring hetero atom, not provided for by groups C07D211/00 - C07D219/00 condensed with carbocyclic rings or ring systems
- C07D221/04—Ortho- or peri-condensed ring systems
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Abstract
The invention relates to a green environmentally-friendly industrial sinomenine extraction and separation method, sinomenine aw material powder as a raw material is added with slaked lime accounting 10% by weight of the raw material for even mixing, then is sprayed to wet with water and placed for a plurality of hours for alkalization, the alkalized material is put into an extracting tank, and added with a certain amount of ethyl acetate solvent for refluxing and extracting for 3 times, the extract in the extracting tank is filtered and sucked into a concentrator for vacuum concentration, the concentrated liquid is placed in the extracting tank, hydrochloric acid is added for adjusting pH to 4-5 for extraction, the hydrochloric acid layer is released, activated carbon is used for decolorization, pH is adjusted to about 2, and the liquid is placed overnight for precipitation of sinomenine hydrochloride. The traditional high toxicity benzene extraction and chloroform extraction processes are substituted by use of ethyl acetate as the extraction solvent, the problems of pollution on the environment and harm on human and animal health of existing technology can be solved, and sinomenine hydrochloride product can be directly obtained without crystallization of a product in a crude extract.
Description
Technical field
The present invention relates to a kind of environmental protection industrialization extraction and separation method of tuduranine.
Background technology
Stem of Orientoine (Sinomenium acutum) is the dry rattan of Menispermaceae Chondodendron plant amedica sinomenium acutum and hair sinomenium acutum, be born in mountain region, be distributed in the ground such as Shaanxi, Sichuan, Guizhou, Hubei, Guangxi, Guangdong, Fujian, Zhejiang, Jiangsu, Anhui, Henan, be used for rheumatic arthralgia, arthroncus, paralysis itch as traditional Chinese medicine, there is effect of dispeling wind and dehumidification, the meridian dredging.Since the twenties in last century, Japanese scholars and domestic scholars are separated and have found tens of kinds of alkaloids from Stem of Orientoine, and prove that tuduranine is main active ingredient wherein, and the content in plant is 0.5% ~ 2%.Pharmacology activity research shows: tuduranine has the multiple pharmacologically actives such as anti-inflammatory, immunosuppression, analgesia, step-down, anti-arrhythmia, is a kind of alkaloid with morphinan structures.To be separated the tuduranine that obtains in Stem of Orientoine for bulk drug, Zhengqing Pharmaceutical Group Corp., Ltd., Hunan Prov. successfully develops and produces the preparation such as ZHENGQINGFENGTONGNING PIAN, sinomenine hydrochloride injection liquid, for clinical treatment rheumatism, rheumatoid arthritis and irregular pulse, and obtain good efficacy; Also useful tuduranine treatment chronic nephritis, anti-oxidant, antitumor, the report of drug rehabilitation and other dosage form research report of tuduranine in recent years; Shanghai Pharmaceutical Inst., Chinese Academy of Sciences with tuduranine be lead compound through modifying for chemical structure modification, have developed have treatment senile dementia active substance, this research at present enters clinical experimental stage.
Along with tuduranine widespread use clinically and multiple physiologically active revealed; the demand of pharmaceutical industries to tuduranine constantly increases in recent years; the large-scale industrial extraction and isolation of tuduranine has become a vital task in the production of medical material medicine, and large-scale production plays active effect to Devoting Major Efforts To Developing Stem of Orientoine plant amedica resource, promotion local economic development.
Abundant Stem of Orientoine plant resources is contained in China particularly Qinling Mountain Areas, and the special weather condition in the Qinling Mountains create the fine quality of Qinling Mountains Stem of Orientoine plant resources, and the content of tuduranine is 1% ~ 2%.In recent years, in order to Devoting Major Efforts To Developing plant amedica resource, promote local economic development, establishing several family in underfooting, Mount Taibai, the Qinling Mountains take Stem of Orientoine as the botanical drug substance company that plant material produces tuduranine.
At present, the extraction and separation process of the In Shanxi Area industrialization tuduranine patented method that generally adopts Chen Chong etc. to deliver in 1996 or optimization method on this basis.In addition, some patents and literature method report is also had, as supersound extraction, CO
2supercritical extraction, column chromatography etc., but because be only suitable for laboratory operation or instrument cost too high and be not suitable for industrially scalable extract.The patent extractive technique that current enterprise generally adopts is: plant material mixes a certain proportion of unslaked lime or white lime after pulverizing, squirt with water and place a few hours and alkalize, be that solvent refluxing extracts 3 to 5 times with benzene in extractor, extracting solution placement through vacuum concentration to inclining on a small quantity and spends the night in concentration tank, tuduranine is that brownish black coarse-grain is separated out, suction filtration is the remaining benzene of dry removing also, tuduranine coarse-grain uses diluted hydrochloric acid dissolution in enamel pot, activated carbon decolorizing, places and separates out white crystals sinomenine hydrochloride.If product after testing purity can carry out recrystallization process not.But the shortcoming that this technique is the most outstanding is the toxicity problem of pollution to environment and benzene, near factory, the special irritating smell of benzene makes us standing, very adverse influence is produced to shop worker and neighbouring resident, also has pollution to groundwater quality, because the volatility of benzene is large, be exposed in air and be easy to diffusion, cause very large pollution to ambient air, humans and animals sucks or a large amount of benzene of skin contact, can cause acute and Chronic Benzene Poisoning.Long-term suction benzene can damage marrow, red blood corpuscle, white corpuscle, platelet counts is reduced, and makes chromosome aberration, thus cause leukemia, even occur aplastic anemia.Research shows: in leukaemic, has and has benzene and organic articles contact history thereof greatly.IARC (IARC) has confirmed that benzene is I class carcinogens.
Advocating low-carbon (LC) life and today of environment protection, preventing pollution, strict control high pollution are that an enterprise can sustainable development basic.China will start toxic Persistent organic pollutants supervisory system in " 12 " period; Chinese Ministry of Environmental Protection will set up persistence organic pollutant and produce, circulates, uses, discharges, disposes Whole Course Management system, and include persistence organic pollutant in surroundings supervisory system.
Summary of the invention
The technical problem that the present invention solves is mainly reflected in two aspects, one be for noxious solvent benzene in existing tuduranine production technique to the pollution of environment and the harm to people and animal, the basis of existing technique adopts the ethyl acetate of environment-protecting asepsis low cost carry out the extraction of tuduranine as solvent; Two is in new solvent extraction process in ethyl acetate concentrated solution in the non crystallized situation of product tuduranine, directly adopts hydrochloric acid to obtain sinomenine hydrochloride.
The technical solution used in the present invention is as follows:
A kind of environmental protection industrialization extraction and separation method of tuduranine, the method with Stem of Orientoine raw material powder for raw material, white lime is added by 10% part by weight of raw material, mix, squirt with water and place a few hours and alkalize, raw material after alkalization is inserted in extractor, add a certain amount of solvent ethyl acetate, refluxing extraction 3 times, extracting solution in extractor carries out vacuum concentration through filtering to suck in concentration tank, concentrated solution is placed in extractor, adding hydrochloric acid adjusts pH to 4 ~ 5 to extract, release salt acid layer, with activated carbon decolorizing, pH is regulated to be about 2, placement is spent the night, separate out sinomenine hydrochloride.
Further, the raw material after alkalization is inserted in extractor, adds ethyl acetate according to the weightmeasurement ratio 1:5g/ml with raw material.
Further, the yield of tuduranine is up to more than 1% of material quantity.
The environmental protection industrialization extraction and separation method of tuduranine provided by the invention, adopt ethyl acetate as Extraction solvent, replace the larger benzene extraction of traditional toxicity and chloroform extraction technique, solve the problem of existing Technology to the pollution of environment and the healthy harm to people and animal, in crude extract, directly can obtain sinomenine hydrochloride product in the non-crystallizable situation of product simultaneously, have technique simple, cost is low, the advantage of safe green.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
The environmental protection industrialization extraction and separation method of the tuduranine of the embodiment of the present invention, a kind of environmental protection industrialization extraction and separation method of tuduranine, with Stem of Orientoine raw material powder for raw material, take Stem of Orientoine raw material powder 100g, 10g white lime is added by 10% part by weight of raw material, mix, squirt with 2 times of water gagings of raw material and place and alkalize for 4 ~ 6 hours, raw material after alkalization is inserted in extractor, add 500ml ethyl acetate as Extraction solvent, refluxing extraction 3 times, each 2 hours, extracting solution in extractor carries out vacuum concentration through filtering to suck in concentration tank, concentrated solution is placed in extractor, adding hydrochloric acid adjusts pH to 4 ~ 5 to extract, release salt acid layer, with activated carbon decolorizing, pH to 2 is adjusted with acid, placement is spent the night, separate out sinomenine hydrochloride.The yield of tuduranine up to more than 1% of material quantity, content more than 95%.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (3)
1. the environmental protection industrialization extraction and separation method of a tuduranine, it is characterized in that: the method with Stem of Orientoine raw material powder for raw material, white lime is added by 10% part by weight of raw material, mix, squirt with water and place a few hours and alkalize, raw material after alkalization is inserted in extractor, add a certain amount of solvent ethyl acetate, refluxing extraction 3 times, extracting solution in extractor carries out vacuum concentration through filtering to suck in concentration tank, concentrated solution is placed in extractor, adding hydrochloric acid adjusts pH to 4 ~ 5 to extract, release salt acid layer, with activated carbon decolorizing, pH is regulated to be about 2, placement is spent the night, separate out sinomenine hydrochloride.
2. the environmental protection industrialization extraction and separation method of a kind of tuduranine according to claim 1, is characterized in that: the raw material after alkalization is inserted in extractor, adds ethyl acetate according to the weightmeasurement ratio 1:5g/ml with raw material.
3. the environmental protection industrialization extraction and separation method of a kind of tuduranine according to claim 1, is characterized in that: the yield of tuduranine is up to more than 1% of material quantity.
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| CN201410462640.4A CN104311489A (en) | 2014-09-12 | 2014-09-12 | Green environmentally-friendly industrial sinomenine extraction and separation method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113209161A (en) * | 2021-05-28 | 2021-08-06 | 湖南农业大学 | Extract of vine fruit of Sinomenium acutum and preparation method and application thereof |
| CN113980920A (en) * | 2021-11-02 | 2022-01-28 | 湖南正清制药集团股份有限公司 | Carbon-carbon double bond reductase and application thereof |
| CN114957118A (en) * | 2021-02-22 | 2022-08-30 | 湖南正清制药集团股份有限公司 | Extraction method of sinomenine hydrochloride |
| CN115308327A (en) * | 2022-08-05 | 2022-11-08 | 南通大学 | Method for quantitatively detecting concentration of demethylsinomenine in blood plasma and detection kit |
| CN115504936A (en) * | 2021-06-22 | 2022-12-23 | 湖南正清制药集团股份有限公司 | Alkalization equipment and method for sinomenine hydrochloride |
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| 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 |
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| 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 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114957118A (en) * | 2021-02-22 | 2022-08-30 | 湖南正清制药集团股份有限公司 | Extraction method of sinomenine hydrochloride |
| CN113209161A (en) * | 2021-05-28 | 2021-08-06 | 湖南农业大学 | Extract of vine fruit of Sinomenium acutum and preparation method and application thereof |
| CN115504936A (en) * | 2021-06-22 | 2022-12-23 | 湖南正清制药集团股份有限公司 | Alkalization equipment and method for sinomenine hydrochloride |
| CN113980920A (en) * | 2021-11-02 | 2022-01-28 | 湖南正清制药集团股份有限公司 | Carbon-carbon double bond reductase and application thereof |
| CN113980920B (en) * | 2021-11-02 | 2023-10-10 | 湖南正清制药集团股份有限公司 | Carbon-carbon double bond reductase and application thereof |
| CN115308327A (en) * | 2022-08-05 | 2022-11-08 | 南通大学 | Method for quantitatively detecting concentration of demethylsinomenine in blood plasma and detection kit |
| CN115308327B (en) * | 2022-08-05 | 2024-01-23 | 南通大学 | Method for quantitatively detecting concentration of norsinomenine in blood plasma and detection kit |
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