Method for separating and preparing echinacoside in herba cistanche

A technology of echinacoside and cistanche, which is applied to the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problems of difficulty in obtaining high-purity samples, low separation efficiency, and cumbersome operations, and achieve The effects of technological innovation and improvement, solvent saving, and short separation time

Inactive Publication Date: 2010-06-02
华美恒盛(北京)科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] At present, the separation of phenylethanol glycosides mostly uses column chromatography, but the operatio

Method used

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  • Method for separating and preparing echinacoside in herba cistanche
  • Method for separating and preparing echinacoside in herba cistanche
  • Method for separating and preparing echinacoside in herba cistanche

Examples

Experimental program
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Effect test

Embodiment 1

[0018] Crush 2.0Kg of Herba Cistanche, extract with 30% ethanol under reflux, dissolve the extract in water, use polyamide column chromatography, elute with water and ethanol, collect 20-40% ethanol eluate, recover the solvent, concentrate under reduced pressure and evaporate to a certain level. Concentration; further purification by medium pressure preparative chromatography using C 18 Column (self-installed), methanol-0.5% acetic acid water (1:1.5, V / V) solution gradient elution, HPLC monitoring, collected samples containing echinacoside, evaporated to dryness;

[0019] A semi-preparative high-speed countercurrent chromatograph was used to separate and prepare echinacoside from the above-mentioned Cistanche cistanche sample using n-butanol-ethyl acetate-ethanol-water system as the solvent. Firstly, the above-mentioned solvent system was arranged in a separatory funnel with a volume ratio of 4:4:1:12, shaken evenly and allowed to stand for stratification. After equilibrating ...

Embodiment 2

[0024] Grind 2.0Kg of Herba Cistanche medicinal material, reflux extraction with 50% ethanol, dissolve the extract in water, use polyamide column chromatography, elute with water and ethanol, collect 20-40% ethanol eluate, recover solvent, concentrate under reduced pressure and steam to a certain Concentration; further purification by medium pressure preparative chromatography using C 18 Column (self-installed), methanol-0.5% acetic acid water (1:2.33, V / V) solution gradient elution, HPLC monitoring, collected samples containing echinacoside, evaporated to dryness;

[0025] A semi-preparative high-speed countercurrent chromatograph was used to separate and prepare echinacoside from the above-mentioned Cistanche cistanche sample using n-butanol-ethyl acetate-ethanol-water system as the solvent. Firstly, the above-mentioned solvent system was arranged in a separatory funnel with a volume ratio of 1.25:1:0.2:4, shaken evenly and allowed to stand for stratification. After equilibr...

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Abstract

The invention relates to a method for separating and preparing echinacoside in herba cistanche. The method comprises the following steps of: dissolving an ethanol extractive of a herba cistanche medicinal material in water; adopting polyamide column chromatography and eluting with water and ethanol; recovering a solvent, decompressing and concentrating; purifying by adopting intermediate-pressure preparative chromatography, wherein a chromatographic column is a C18 column, methanol and 0.5 percent acetic acid aqueous solution are used as an eluant, and the volume ratio of the methanol to the 0.5 percent acetic acid aqueous solution is (1-2.5):(4-1.5); HPLC monitoring; collecting a sample containing the echinacoside and drying by distillation; separating the sample containing the echinacoside by adopting a high speed counter current chromatograph; arranging a solvent system containing n-butyl alcohol, ethylacetate, ethanol and water in a liquid separating funnel; and sufficiently shaking the solvent and then standing still for 12 hours for layering, wherein an upper phase is used as a fixed phase, a lower phase is used as a flowing phase, and the volume ratios of the n-butyl alcohol to the ethylacetate to the ethanol to the water is (1-5):(1-5):(0.2-1):(5-10). The method is used for preparing the echinacoside, and the purity of the prepared echinacoside is higher than 98 percent.

Description

Technical field: [0001] The invention relates to a method for preparation and separation of countercurrent chromatography, in particular to a method for separating and preparing high-purity echinacoside from ethanol crude extract of Cistanche deserticola by using high-speed countercurrent chromatography. Background technique: [0002] Herba Cistanche (Herba Cistanche) is a well-known traditional Chinese tonic medicine. The Cistanche deserticola recorded in the 2005 edition of the "Chinese Pharmacopoeia" is the dried flesh of Cistanche deserticoal Y.C.Ma and Cistanche tubulosa (Schrenk) R.Wight. The stem has the functions of invigorating the kidney and strengthening yang, replenishing essence and marrow, nourishing blood and moistening dryness, pleasing color and prolonging life. The application rate in anti-aging and anti-aging prescriptions is second only to ginseng, and it has excellent medicinal value, known as "desert ginseng". [0003] Modern research shows that the ma...

Claims

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Application Information

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IPC IPC(8): C07H15/18C07H1/08
Inventor 张天佑孙庆武张文晋王晓
Owner 华美恒盛(北京)科技有限公司
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