CN103435630A - Preparation method of liatrin - Google Patents

Abstract

The invention discloses a preparation method of liatrin, which is high in extraction efficiency and less in pollution. The method comprises the following steps that a, gutenbergia cordifolia leaves are taken, dried, subjected to impurity removal, smashed into 20-80 meshes, and placed in a CO2 supercritical extraction pot for extraction with the CO2 flow of 1-5ml/min/g raw material, the extraction temperature of 30-60 DEG C, the pressure of 20-30Mpa, and the extraction time of 1-4h, and a crude extract is obtained; and b, the crude extract is subjected to heat dissolution with a 30-40% methanol solution with the quantity of 2-3 times that of the crude extract, is added to macroporous resin to be absorbed, and eluted by a 50% methanol solution and an 80% methanol solution sequentially; an eluant of the 80% methanol solution is collected, and subjected to pressure reduction concentration; concentrated liquid is extracted by a methylene chloride solution; and extract liquid is concentrated to be 1/10 of the volume, refrigerated, crystallized, subjected to crystal substance filtration, recrystallized with the methanol solution, and dried to form liatrin. With the adoption of the method to produce liatrin, technological operation is simple; the obtained product is high in purity; and industrial production is facilitated.

Description

A kind of preparation method of liatrin

Technical field

The invention belongs to biological technical field, be specifically related to a kind of preparation method of liatrin.

Background technology

Liatrin is the lactone material, CAS 34175-79-6, and molecular weight is C22H126O8, molecular weight is 418.4, molecular structural formula:

Liatrin is needle crystal, and fusing point 130-132 ° has anti-inflammatory, antitumor action.

By literature search, the liatrin preparation method adopts the organic reagent extraction to separate with silicagel column more.This class methods extraction efficiency is low, seriously polluted, is not suitable for suitability for industrialized production.

Summary of the invention

The technical problem to be solved in the present invention is to provide a kind of preparation method of simple to operate, liatrin that product purity is high.

The present invention is achieved by the following technical solutions:

A kind of preparation method of liatrin is characterized in that comprising the following steps:

1) get the dry impurity elimination of prairie pine herb and pulverize the 20-80 order, being placed in CO2 supercritical extraction tank extracts, pass into liquid CO 2, flow is the 1-5ml/min/g raw material, passes into 90% ethanol simultaneously and does entrainment agent, and flow is 1-3ml/min/g, raw material abstraction temperature 30-60 ℃, pressure 15-30Mpa, extraction time 1-4h, resolve to obtain extract;

2) 20%-40% ethanolic soln thermosol for above-mentioned extract, add in macroporous resin column and adsorb, and first with 20 times of amount 40% wash-outs, then uses 20 times of 70% ethanolic soln wash-out, and the elutriant concentrating under reduced pressure, place crystallization, leaches crystallisate with the dehydrated alcohol recrystallization and get final product.

Extracting pressure 22MPa in described step 1).

Described step 2) a kind of in the optional AB-8 of macroporous resin model in, D101, HZ816, HPD400.

Adopt technique scheme to produce liatrin, extraction efficiency is high, and product purity is high, and environmentally friendly, is easy to large production.

Embodiment

below in conjunction with specific embodiment, the invention will be further described.

Embodiment 1:

Get prairie pine herb 5kg, 60 orders are pulverized in dry impurity elimination, be placed in CO2 supercritical extraction tank, pass into liquid CO 2, flow is the 2ml/min/g raw material, pass into 90% ethanol simultaneously and do entrainment agent, flow is 2ml/min/g, 40 ℃ of raw material abstraction temperature, pressure 22Mpa, extraction time 2h, resolve, 30% ethanolic soln thermosol for extract, add in the AB-8 macroporous resin column and adsorb, first with 20 times of amount 40% wash-outs, use again 20 times of 70% ethanolic soln wash-out, the elutriant concentrating under reduced pressure, place crystallization, leach crystallisate dehydrated alcohol recrystallization, obtain liatrin 23g, through HPL, detect, content 98.4%.

Embodiment 2:

Get prairie pine herb 5kg, 80 orders are pulverized in dry impurity elimination, be placed in CO2 supercritical extraction tank, pass into liquid CO 2, flow is the 3ml/min/g raw material, pass into 90% ethanol simultaneously and do entrainment agent, flow is 1ml/min/g, the raw material abstraction temperature 45 C, pressure 25Mpa, extraction time 12h, resolve, 20% ethanolic soln thermosol for extract, add in the D101 macroporous resin column and adsorb, first with 20 times of amount 40% wash-outs, use again 20 times of 70% ethanolic soln wash-out, the elutriant concentrating under reduced pressure, place crystallization, leach crystallisate dehydrated alcohol recrystallization, obtain liatrin 18g, through HPL, detect, content 98.7%.

Embodiment 3:

Get prairie pine herb 5kg, 40 orders are pulverized in dry impurity elimination, be placed in CO2 supercritical extraction tank, pass into liquid CO 2, flow is the 1ml/min/g raw material, pass into 90% ethanol simultaneously and do entrainment agent, flow is 1ml/min/g, 40 ℃ of raw material abstraction temperature, pressure 20Mpa, extraction time 3h, resolve, 30% ethanolic soln thermosol for extract, add in the HZ816 macroporous resin column and adsorb, first with 20 times of amount 40% wash-outs, use again 20 times of 70% ethanolic soln wash-out, the elutriant concentrating under reduced pressure, place crystallization, leach crystallisate dehydrated alcohol recrystallization, obtain liatrin 24g, through HPL, detect, content 98.1%.

Embodiment 4:

Get prairie pine herb 5kg, 20 orders are pulverized in dry impurity elimination, be placed in CO2 supercritical extraction tank, pass into liquid CO 2, flow is the 3ml/min/g raw material, pass into 90% ethanol simultaneously and do entrainment agent, flow is 2ml/min/g, the raw material abstraction temperature 45 C, pressure 15Mpa, extraction time 2h, resolve, 30% ethanolic soln thermosol for extract, add in the HPD400 macroporous resin column and adsorb, first with 20 times of amount 40% wash-outs, use again 20 times of 70% ethanolic soln wash-out, the elutriant concentrating under reduced pressure, place crystallization, leach crystallisate dehydrated alcohol recrystallization, obtain liatrin 21g, through HPL, detect, content 97.8%.

Claims (3)

1. the preparation method of a liatrin is characterized in that comprising the following steps:

1) get the dry impurity elimination of prairie pine herb and pulverize the 20-80 order, being placed in CO2 supercritical extraction tank extracts, pass into liquid CO 2, flow is the 1-5ml/min/g raw material, passes into 90% ethanol simultaneously and does entrainment agent, and flow is 1-3ml/min/g, raw material abstraction temperature 30-60 ℃, pressure 15-30Mpa, extraction time 1-4h, resolve to obtain extract;

2) 20%-40% ethanolic soln thermosol for above-mentioned extract, add in macroporous resin column and adsorb, and first with 20 times of amount 40% wash-outs, then uses 20 times of 70% ethanolic soln wash-out, and the elutriant concentrating under reduced pressure, place crystallization, leaches crystallisate with the dehydrated alcohol recrystallization and get final product.

2. the preparation method of liatrin according to claim 1, is characterized in that the extracting pressure 22MPa in described step 1).

3. the preparation method of liatrin according to claim 1, is characterized in that described step 2) in the optional AB-8 of macroporous resin model, D101, HZ816, HPD400 in a kind of.