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Process for extracting schizandrin A from schizandra

A technology of Schisandrin A and Schisandra chinensis, applied in ether separation/purification, ether preparation, organic chemistry and other directions, can solve the problems of low product purity, high equipment requirements, difficult to control operating conditions, etc., and achieve high product purity and separation effect. Good, fast extraction effect

Inactive Publication Date: 2011-02-16
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The traditional extraction methods of schisandrin A include alcohol extraction, chloroform extraction and hot water extraction. Fadosol solvent is a solvent system developed in recent years, mainly composed of 1,1,1,2-tetrafluoroethane, Liu Ben et al. Extraction of Schizandrin from Schisandra chinensis by Fadosol solvent [J]. Chinese Patent Medicine, 2000, 22(7): 507-509." Using low-pressure cold extraction device to extract Schizandrin A, the product is not pure and still needs further purification. Compared with traditional extraction methods, this method is more expensive
Yang Subei's "Study on the Technology of Supercritical Fluid Extraction of Lignans and Other Components in Schisandra Fructus" discloses the method of supercritical CO2 extraction of lignans in Schisandra chinensis, but supercritical CO2 extraction technology is a high-pressure technology, which requires high equipment and is expensive , not conducive to mass production
Chinese patent (Application No. 200910242188.X) "Separation and preparation method of Schisandra chinensis monomer components", the disclosed method is to extract the ethanol extract of Schisandra chinensis with petroleum ether, use silica gel column chromatography for the petroleum ether extract, and use petroleum ether-acetic acid Ethyl elution, HPLC monitoring, collect the elution fraction crude extract A, crude extract B; eluent petroleum ether-ethyl acetate volume ratio is 3-5:1; crude extract A and crude extract B Separated by high-speed countercurrent chromatography to obtain schisandrin, schisandrin A, schisandrin B, schisandrin C, schisandrin A, schisandrin B and schisandrin ester B monomers. This method does not need to use solid fillers and has no irreversible adsorption. There is no loss and pollution of samples, but the operating conditions are difficult to control

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Grind Schisandra chinensis to 40 mesh, take 1.5 kg and use 5 times the quality of medicinal materials to ultrasonically extract petroleum ether for 2 times, each time for 1 hour, collect the extract, filter under normal pressure, and use 2 times the volume of 40% methanol (alkaline adjustment ph8) Extract 3 times, combine the petroleum ether layer, wash with water until neutral, use a rotary evaporator to concentrate under reduced pressure to obtain 60 g of the total lignan extract, take 1 kg of silica gel and 200 g of alumina, mix it evenly and pack it into a column, and the above-mentioned total lignan extract Mix the sample with 180g of 100-150 mesh alumina, put it on the column, elute with chloroform, combine the fractions rich in schisandrin A, concentrate with a rotary evaporator, dry at 40°C, and mix with an equal amount of 250-300 mesh silica gel , go on silica gel alumina column chromatography again, elute with 98:2 chloroform-methanol solution, collect eluate, ...

Embodiment 2

[0028] Schisandra chinensis is crushed to 60 meshes, 1.5 kg is extracted 3 times with petroleum ether with 8 times the quality of the medicinal materials, and each time for 2 hours, the extract is collected, filtered at normal pressure, diluted with water, and diluted with 55% ethanol (alkali) with 3 times the volume. Adjust pH to 8.5) and extract 4 times, combine the petroleum ether layers, wash with water until neutral, concentrate under reduced pressure with a rotary evaporator to obtain 55 g of the total lignan extract, take 1 kg of silica gel and 150 g of alumina, mix them evenly and pack them into a column, and put the above-mentioned lignin The total lipid extract was mixed with 200g of 150-200 mesh alumina, put on the column, eluted with chloroform, combined the fractions rich in schisandrin A, concentrated with a rotary evaporator, dried at 40°C, and then mixed with an equivalent amount of 250- Mix the 300 mesh silica gel evenly, apply the silica gel alumina column chr...

Embodiment 3

[0030] Schisandra chinensis is crushed to 50 meshes, 3 kg is ultrasonically extracted 3 times with petroleum ether with 7 times the quality of medicinal materials, each time for 1.2 h, the extract is collected, filtered at normal pressure, diluted with water, and 75% methanol (alkali) with 3 times the volume Adjust ph9) and extract 5 times, combine the petroleum ether layer, wash with water until neutral, concentrate under reduced pressure with a rotary evaporator to obtain 72g of the total lignan extract, take 2.4kg of silica gel and 240g of alumina and mix them evenly for column packing. The total extract was mixed with 250g of 100-150 mesh alumina, put on the column, eluted with chloroform, combined the fractions rich in schisandrin A, concentrated with a rotary evaporator, dried at 40°C, and then mixed with an equivalent amount of 200-250 The silica gel was mixed evenly, and the silica gel alumina column chromatography was applied again, and 95:2 chloroform-methanol solutio...

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PUM

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Abstract

The invention relates to a process for extracting schizandrin A from schizandra, which is characterized by preparing total lignan extracts through ultrasonic-assisted petroleum ether extraction and alkali-alcohol back extraction, carrying out mixed column chromatography on silica gel and alumina twice, eluting silica gel and alumina and recovering the solvent, and recrystallizing and drying petroleum ether-acetone or cyclohexane-ethanol, thus obtaining the schizandrin A. The process has high specificity.

Description

Technical field: [0001] The invention belongs to the field of natural plant extraction, and relates to a process for extracting schisandrin from schisandra chinensis. Background technique: [0002] Schisandra chinensis, commonly known as Zanthoxylum bungeanum, Scale Duozi, Medicinal Schisandra, Mianteng, Wumeizi, etc., has the effects of astringent and astringent, nourishing qi and promoting body fluid, nourishing kidney and calming heart. For chronic cough and shortness of breath, nocturnal spermatorrhea, enuresis, frequent urination, chronic diarrhea, spontaneous sweating, night sweats, thirsty body fluid wounds, shortness of breath and arteries, internal heat and quenching thirst, palpitations and insomnia. The main chemical components are deoxyschizandrin (de-oxyschizandrin), schisandrin (schizandrin), neoschizandrin (neoschizandrin), schizandrol (schizan-drol), schisandrin (schisantherin, gomisin), etc., which are active ingredients for the treatment of hepatitis For S...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/38C07C43/21C07C41/36
Inventor 刘东锋郭琴杨成东
Owner NANJING ZELANG MEDICAL TECH
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