CN104693253A

CN104693253A - Industrial preparation method for high-purity 6'-O-trans-cinnamyl catalpol

Info

Publication number: CN104693253A
Application number: CN201510140963.6A
Authority: CN
Inventors: 贺灵剑; 刘培冉; 杨涛; 刘文卉; 李啸然; 孙士青
Original assignee: JINAN DONGYUAN BIOMEDICAL TECHNOLOGY Co Ltd
Current assignee: JINAN DONGYUAN BIOMEDICAL TECHNOLOGY Co Ltd
Priority date: 2015-03-30
Filing date: 2015-03-30
Publication date: 2015-06-10

Abstract

The invention relates to a preparation method for high-purity 6'-O-trans-cinnamyl catalpol. Raw materials are residual extract obtained after 10-vanilla bean acyl catalpol is prepared through the 'method for preparing 10-vanilla bean acyl catalpol' introduced in the patent (patent number: 201110400683.6), and after primary separation, elution separation is carried out with aluminum oxide as the stationary phase and an ethanol-water system of a certain proportion as an elution solvent. The 6'-O-trans-cinnamyl catalpol with the purity not lower than 90% is obtained, and a separation and purification method of the 6'-O-trans-cinnamyl catalpol is expanded. A normal pressure method is adopted, cost is low, efficiency is high, and the method is especially suitable for large-scale industrial production.

Description

The preparation of industrialization of the trans cinnamyl Catalpol of high purity 6 '-O-

Technical field

The present invention relates to one chromatographic aluminium oxide is the method that sorbent material carries out that normal pressure column chromatography obtains the trans cinnamyl Catalpol of high purity 6 '-O-, belongs to medical art.

Background technology

Rhizoma Picrorhizae is the dry rhizome of goatweed Rhizoma Picrorhizae, there are heat-clearing, dehumidifying, improving eyesight, hepatic cholagogic, treatment pediatric epilepsy scared, infantile malnutrition due to digestive disturbances or intestinalparasites, rush down dysentery, main component in Rhizoma Picrorhizae is iridoids, cucurbitacine and phenolic glycoside class, the topmost composition of iridoids is the trans cinnamyl Catalpol of 6 '-O-and 10-fragrant pod acyl Catalpol.

The trans cinnamyl Catalpol of 6 '-O-has hepatic cholagogic effect and the provide protection to neural cell injury.

The patent of the trans cinnamyl Catalpol of existing preparation 6 '-O-has two, one (the patent No.: 201310618996.8) major technique carries out the obtained trans cinnamyl Catalpol of highly purified 6 '-O-of separation for utilizing preparation liquid phase, preparation liquid phase applied sample amount is little, efficiency is low, consumptive material is expensive, adds the production cost of the trans cinnamyl Catalpol of 6 '-O-.(patent No.: 200710164321.5) solvent for use is acetone, poisonous, for the residual inspection in later stage makes troubles for another patent.This technology adopts normal pressure method, and cost is low, and efficiency is high, is specially adapted to large-scale industrial production.

The structural formula of the trans cinnamyl Catalpol of 6 '-O-is:

Summary of the invention

Adopt the patent (patent No.: it is raw material that method prepared by the 10-that 201110400683.6) introduces fragrant pod acyl Catalpol prepares remaining extract after 10-fragrant pod acyl Catalpol, carry out silica gel column chromatography separation, by ethyl acetate: the mixed solvent that ethanol (25:1--4:1) is made into carries out gradient elution, obtains the trans cinnamyl Catalpol of 6 '-O-that purity is not less than 70%.

Aluminum oxide dry column-packing, be not less than the 6 '-O-trans cinnamyl Catalpol extract of 70% for raw material with purity, with anhydrous alcohol solution, wet method loading, first uses dehydrated alcohol wash-out, is eluted to colourless, then uses ethanol (dehydrated alcohol--80%) to carry out gradient elution.Collect elutriant, merge the wash-out drying under reduced pressure of 6 '-O-trans cinnamyl Catalpol normalized area more than 90% and namely obtain the trans cinnamyl Catalpol of high purity 6 '-O-.

Embodiment

Following examples illustrate the present invention, but scope is not limited to the content that the following example comprises.

1). dress post: take neutral alumina 2kg, dry column-packing.

2). molten sample: get 6 '-O-trans cinnamyl Catalpol purity be 73% solid 100g be dissolved in dehydrated alcohol, the consumption of ethanol is got the trans cinnamyl Catalpol of 6 '-O-by dissolving.

3). loading: trans for 6 '-O-of dissolve with ethanol cinnamyl Catalpol, slowly add alumina column with separating funnel, keeps chromatography column post bed surface smooth.

4). wash-out: use dehydrated alcohol wash-out, every 400ml collects once, be washed till effluent liquid colourless, change 95% ethanol into wash, front 1600-2000ml essential substance is impurity, is next exactly the trans cinnamyl Catalpol of highly purified 6 '-O-, normalized area more than 90%, collecting amount is about 6000ml, 6 '-O-trans cinnamyl Catalpol normalized area is more below lower, collects and manages elsewhere.

5) get the effluent liquid recycling design that step 4 is collected, namely evaporated under reduced pressure obtains high purity 6 '-O-trans cinnamyl Catalpol powder 50g, purity 93%.

Claims

1. normal pressure column chromatography prepares the trans cinnamyl Catalpol of high purity 6 '-O-, it is characterized in that, be not less than the trans cinnamyl Catalpol of 6 '-O-of 70% for raw material with content under condition of normal pressure, chromatographic aluminium oxide Column preparation content is not less than the trans cinnamyl Catalpol of 90% high purity 6 '-O-.

2. high purity 6 '-O-trans cinnamyl Catalpol preparation method as described in claim 1, it is characterized in that, condition used is normal pressure.

3. as described in claim 1 high purity 6 '-O-trans cinnamyl Catalpol preparation method, is characterized in that, the ethanol that the method comprises with concentration is not less than 80% is eluting solvent.

4. high purity 6 '-O-trans cinnamyl Catalpol preparation method as described in claim 1, is characterized in that, chromatographic aluminium oxide used is neutral, acid or alkaline.