Method for preparing salvianolic acid B and rosmarinic acid by adopting high-speed counter-current chromatography separation and purification process

A high-speed countercurrent chromatography, rosmarinic acid technology, applied in the field of natural medicine separation, can solve the problems of time-consuming and laborious, polluting the environment, irreversible adsorption, etc., and achieve the effects of good separation effect, less solvent consumption and easy operation.

Active Publication Date: 2014-09-10
ANHUI YONSENT PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The existing technology generally adopts traditional separation methods such as ordinary chromatographic column method and recrystallization to separate effective

Method used

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  • Method for preparing salvianolic acid B and rosmarinic acid by adopting high-speed counter-current chromatography separation and purification process
  • Method for preparing salvianolic acid B and rosmarinic acid by adopting high-speed counter-current chromatography separation and purification process
  • Method for preparing salvianolic acid B and rosmarinic acid by adopting high-speed counter-current chromatography separation and purification process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] 1. Take 100g of Salvia miltiorrhiza and crush it into a coarse powder, add 1000mL of 50% ethanol by heating and reflux for extraction twice, extract for 1 hour each time, combine the extracts and filter, cool to room temperature, and depressurize the filtrate to alcohol-free with a rotary evaporator , to obtain ethanol extract 62g, its high performance liquid chromatogram is as follows figure 1 shown.

[0034] 2. After dispersing 3.6g ethanol extract with 30mL water, add it to HPD300 macroporous adsorption resin column chromatography. % ethanol → 5 times column volume 50% ethanol → 5 times column volume 60% ethanol → 5 times column volume 95% ethanol solution elution, collect the ethanol eluate containing the target product salvianolic acid B, rosmarinic acid, reduce Concentrate under pressure to no alcohol, dry to obtain the mixed crude extract of salvianolic acid B and rosmarinic acid, the HPLC figure is shown in figure 2 . (% means volume fraction)

[0035] 3. U...

Embodiment 2

[0042] 1. Extraction of Salvia miltiorrhiza and separation by macroporous resin chromatography are the same as in Example 1.

[0043] 2. Use high-speed countercurrent chromatography to separate and purify the crude extract: take n-hexane, ethyl acetate, methanol, and water, mix them in a volume ratio of 3:7:1:9, mix them well and let stand, separate the upper and lower phases, and take the upper and lower phases. The phase is the stationary phase, and the lower phase is the mobile phase. Fill the stationary phase with the multi-layer coil separation column of the high-speed countercurrent chromatograph, turn on the high-speed countercurrent chromatograph, and adjust the speed to 800r min -1 , inject mobile phase, mobile phase flow rate 1.8mL min -1 , when the mobile phase obviously flows out, take 172mg of the mixed crude extract of salvianolic acid B and rosmarinic acid, dissolve it in 10mL of the mixture of upper phase and lower phase with a volume ratio of 1:1, and inject t...

Embodiment 3

[0046] 1. Extraction of Salvia miltiorrhiza and separation by macroporous resin chromatography are the same as in Example 1.

[0047] 2. Use high-speed countercurrent chromatography to separate and purify the crude extract: Take n-hexane, ethyl acetate, acetone, and water, mix them in a volume ratio of 3:7:1:9, and let stand after mixing fully. Separate the upper and lower phases, and take the upper and lower phases. The phase is the stationary phase, and the lower phase is the mobile phase. Fill the stationary phase with the multi-layer coil separation column of the high-speed countercurrent chromatograph, turn on the high-speed countercurrent chromatograph, and adjust the speed to 800r min -1 , inject mobile phase, mobile phase flow rate 1.8mL min -1 , when the mobile phase obviously flows out, take 156mg of the mixed crude extract of salvianolic acid B and rosmarinic acid, dissolve it in 10mL of the upper phase and lower phase mixed solution with a volume ratio of 1:1, and ...

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Abstract

The invention discloses a method for preparing salvianolic acid B and rosmarinic acid by adopting a high-speed counter-current chromatography separation and purification process. The method comprises the following steps: grinding salvia miltiorrhiza, performing ethanol extraction, enriching through macroporous adsorption resin to obtain a crude extract, and performing high-speed counter-current chromatography separation on the crude extract by a high-speed counter-current solvent system consisting of solvents A, B, C and D to prepare salvianolic acid B and rosmarinic acid respectively, wherein the volume ratio of the solvent A to the solvent B to the solvent C to the solvent D is (1-5) to (5-10) to (1-5) to (1-10); the solvent A is methanol, ethanol, n-hexane or iso-hexane; the solvent B is ethyl acetate, propyl acetate or n-butyl acetate; the solvent C is methanol, ethanol or acetone; the solvent D is water; an upper phase is a stationary phase; a lower phase is a mobile phase. According to the method, the salvianolic acid B and the rosmarinic acid are prepared by adopting the high-speed counter-current chromatography process, inreversible adsorption is not existent, and the sample loss is avoided; the method has the characteristics of having a good separation effect and being low in solvent consumption, pollution-free, efficient and quick.

Description

technical field [0001] The invention belongs to the field of separation of natural medicines, and relates to a method for separating and purifying salvianolic acid B and rosmarinic acid, in particular to a method for separating and purifying high-purity salvianolic acid B and rosmarinic acid by high-speed countercurrent chromatography. Background technique [0002] Salvia miltiorrhiza is the dry root of Salvia miltiorrhiza Bge., a plant in the Labiatae family. It has the medicinal effects of promoting blood circulation, promoting menstruation, removing blood stasis and relieving pain, and clearing heart and annoyance. The chemical components of Danshen are mainly water-soluble salvianolic acids and fat-soluble tanshinones. Salvianolic acid B has strong antioxidant and oxygen free radical scavenging activities. Rosmarinic acid is a natural antioxidant with anti-inflammatory and antioxidant activities. [0003] Salvianolic acid B molecular structure formula is as follows: ...

Claims

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Application Information

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IPC IPC(8): C07D307/86C07C69/732C07C67/48
CPCC07C67/48C07D307/86C07C69/732
Inventor 李行诺童胜强颜继忠张文强
Owner ANHUI YONSENT PHARMA
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