Novel technique for preparing schizandrol A and schizandrol B

A technology of schisandrin B and schisandrin A, applied in the field of medicine, can solve problems such as quality decline, low purity, rising price, etc., and achieve the effects of alleviating shortage, simple process and convenient operation.

Active Publication Date: 2009-08-12
SHENYANG PHARMA UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Chinese patent specification CN1817839A discloses a process for extracting schisandrin A. The method is to use the fruit of Schisandra chinensis as a raw material, through solvent extraction, and after the extract is separated by column chromatography, the purity of the obtained schisandrin A is only 50% or More than 50% is light green powder, the higher the purity of lignans, the lighter or colorless its color should be, so it can be seen that the purity of its method is not high, and at present, due to the large market demand of Schisandra chinensis, far Unable to meet the requirements of the domestic and foreign markets, there have been extinct vine harvesting and destruction of resources. In some areas, the phenomenon of plundering greens has generally occurred, causing the resources of Schisandra chinensis to be damaged to varying degrees, resulting in the reduction of available resources of Schisandra chinensis and the quality. Falling, rising prices
[0006] Schizandrin B and Schizandrin A chemical reference substances sold in the market are all extracted from Schisandra fruit, and the invention of Schizandrin B and Schisandrin A chemical reference substances extracted from Schisandrin leaves has not been reported.

Method used

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  • Novel technique for preparing schizandrol A and schizandrol B
  • Novel technique for preparing schizandrol A and schizandrol B
  • Novel technique for preparing schizandrol A and schizandrol B

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 5.2 kg of schisandra leaves were crushed, added with 80% acetone and extracted under reflux for 3 times, each time for 2 hours, filtered, and the combined filtrates were concentrated under reduced pressure to 3.5 L of medicinal solution with a density of 0.982. Add an equal volume of petroleum ether for extraction 6 times, and concentrate the petroleum ether layer to dryness under reduced pressure to obtain 150 g of the extract. The extract is subjected to silica gel column chromatography, and the volume ratio of dichloromethane-methanol (300:0.5—300:5) is Gradient elution of the mixed solution, roughly divided into 6 sections, TLC detection, collecting the second section rich in schisandra alcohol B, and then performing a second silica gel column chromatography, using cyclohexane-ethyl acetate (10:1- 1:1) mixed solution with a volume ratio of 1:1) was eluted, TLC was detected, and the part rich in schisandra alcohol B was collected, and recrystallized repeatedly with me...

Embodiment 2

[0020] 5.2 kg of schisandra leaves were crushed, added with 75% ethanol, heated and refluxed for 3 times, 2 hours each time, filtered, and the combined filtrate was concentrated under reduced pressure to 4.5 L of medicinal solution with a density of 0.982. An equal volume of petroleum ether was added for extraction 6 times, and the petroleum ether layer was concentrated to dryness under reduced pressure to obtain 203 g of the extract. The extract was subjected to silica gel column chromatography, and the volume ratio of dichloromethane-methanol (300:0.5—300:5) was Gradient elution of the mixed solution, roughly divided into 6 sections, TLC detection, collecting the second section rich in schisandra alcohol B, and then performing a second silica gel column chromatography, using cyclohexane-ethyl acetate (10:1- 1:1) mixed liquid with a volume ratio of 1:1) was eluted, TLC was detected, and the part rich in Schisandrin B was collected, petroleum ether-methanol-water was recrystall...

Embodiment 3

[0022] 5.2 kg of schisandra leaves were crushed, added with 75% ethanol, heated and refluxed for 3 times, 2 hours each time, filtered, and the combined filtrate was concentrated under reduced pressure to 4.5 L of medicinal solution with a density of 0.982. Adsorbed on the HPD100 macroporous resin on the liquid medicine, and eluted with water, 30%, and 40-90% ethanol successively, collected 40-90% ethanol eluate, recovered ethanol and evaporated to dryness in a water bath to obtain 160.8 g of eluate, and washed Carry out silica gel column chromatography, and use dichloromethane-methanol (300:0.5—300:5) volume ratio mixed solution gradient elution, roughly divide into 6 sections, TLC detection, collect the second phase rich in schisandra alcohol B Section part, then perform secondary silica gel column chromatography, elute with the mixed solution of cyclohexane-ethyl acetate (10:1-1:1) volume ratio, TLC detection, collect the part rich in schisandra alcohol B, Repeated recrystal...

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PUM

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Abstract

The invention belongs to the field of medical technology and discloses a new preparation technique of schizandrol B and schizandrol A in schisandra chinensis baill leaves. The technique comprises the steps: schisandra chinensis baill leaves are taken as raw material, ground and then processed by one or more technique(s) in solvent extraction method, organic solvent extraction method, resin adsorption method, normal phase column chromatography, reversed-phase column chromatography and the like, namely, the schisandra chinensis baill leaves are taken as raw material, extracting solution containing the schizandrol A and the schizandrol B is extracted by organic solvent; after extract is processed by repeated column chromatographic separation, the flowing parts containing the schizandrol A and the schizandrol B are collected, and the schizandrol A and the schizandrol B are obtained after repeated recrystallization of the condensate; the purities of the schizandrol A and the schizandrol B can be more than 98% by HPLC detection. The preparation method has simple technique, stable purity and good reproduction quality, can be used for replacing shizandra fruit to extract and prepare standard product, fully utilizes the resource of shizandra and relieve the situation that the supply of the shizandra fruit is not adequate to the demand.

Description

technical field [0001] The invention belongs to the technical field of medicine, and relates to a new process for preparing schisandra alcohol A and schisandra alcohol B in large quantities. The process uses schisandra leaves as raw materials instead of commonly used fruits as raw materials. Background technique [0002] 1. Schisandra leaves are Schisandra chinensis (Turcz.) Bill., Schisandra sphenanthera Rehd.et Wils., Kadsura interior A.c.Smith., K.heteroclita (Roxb. ) Craib., the dried leaves of Schisandra viridis A.C. Smith, Schisandra pubescens Hemsl. et Wils., Schisandra sphaerandraStapf. [0003] 2. Foreign scholars applied high-efficiency liquid to compare the CO of Schisandra cotyledon 2 The supercritical extract was analyzed and found to contain the same lignans as Schisandra fruit, schisandrol A, alcohol B, A, B, C and gomisin N (Journal of Chromatography B, 770 (2002) 283-289 ). [0004] Schisandrin A, also known as schizandrin; Schizandrin B, also known as g...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/253C07D317/70C07C41/36C07C41/38C07C41/40A61P1/00A61P9/00A61P25/28A61P15/00A61P39/06A61P17/00
CPCY02P20/54
Inventor 殷军张娜刘志惠周正圆
Owner SHENYANG PHARMA UNIVERSITY
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