Process for preparing high-purity rhodioloside

A salidroside, high-purity technology is applied in the field of separation and preparation of high-purity salidroside, which can solve the problems of complicated operation, low product purity and recovery rate, etc., and achieves solvent saving, no sample loss, and high recovery rate. Effect

Inactive Publication Date: 2002-08-28
北京天纯维通生物技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation of high-purity products is mainly completed by crystallization and preparative high-pressure liquid chromatography. The operation is often cumbersome, and the purity and recovery of the product are low due to the adsorption and denaturation of the sample by the solid support or carrier.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Preparation of salidroside with a purity higher than 98% using ethyl acetate-n-butanol-water and chloroform-methanol-isopropanol-water two-solvent system: using a semi-preparative high-speed countercurrent chromatograph equipped with an NS-1007 pump , 20ml injection valve, polytetrafluoroethylene column, the column volume is 240ml, 8823A-UV ultraviolet detector, Yokogawa 3057 portable recorder. Before sample injection, fill the entire column with stationary phase, adjust the speed of the main engine to 800rpm, and pump the mobile phase into the column at a flow rate of 2.0ml / min. Detector UV spectrum to receive target components. The preparation of salidroside is carried out in two steps: (1) ethyl acetate-n-butanol-water with a volume ratio of 1:2:3 is miscible in a separatory funnel, shaken up and allowed to stand for stratification, and take Its upper layer solution (upper phase) is the stationary phase, and the lower layer solution (lower phase) is the mobile phase...

Embodiment 2

[0015] Use ethyl acetate-isobutanol-acetone-water and chloroform-methanol-water two-solvent system to prepare salidroside with a purity higher than 98%: use a semi-preparative high-speed countercurrent chromatograph equipped with an NS-1007 pump, 20ml Injection valve, polytetrafluoroethylene column, column volume is 240ml, 8823A-UV ultraviolet detector, Yokogawa 3057 portable recorder. Before sample injection, fill the entire column with stationary phase, adjust the speed of the main engine to 800rpm, and pump the mobile phase into the column at a flow rate of 2.0ml / min. Detector UV spectrum to receive target components. The preparation of salidroside is carried out in two steps: (1) ethyl acetate-isobutanol-acetone-water with a volume ratio of 5:40:1:60 is miscible in a separatory funnel, shaken up and allowed to stand Layered, the upper layer solution (upper phase) is taken as the stationary phase, and the lower layer solution (lower phase) is used as the mobile phase. Dis...

Embodiment 3

[0017] Preparation of salidroside with a purity higher than 98% using n-butanol-water and dichloromethane-isopropanol-chloroform-methanol-water two-solvent systems: using a semi-preparative high-speed countercurrent chromatograph equipped with NS-1007 pumps , 20ml injection valve, polytetrafluoroethylene column, the column volume is 240ml, 8823A-UV ultraviolet detector, Yokogawa 3057 portable recorder. Before sample injection, fill the entire column with stationary phase, adjust the speed of the main engine to 800rpm, and pump the mobile phase into the column at a flow rate of 2.0ml / min. Detector UV spectrum to receive target components. The preparation of salidroside is carried out in two steps: (1) n-butanol-water miscibility of 45:53 in volume ratio is mixed in a separatory funnel, after shaking up, the layering is left to stand, and the upper layer solution (upper phase) is taken. ) is a stationary phase, and the lower floor solution (lower phase) is a mobile phase. Diss...

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Abstract

A process for preparing high-purity rhodioloside from natural rhodiola rosea by high-speed counter-current chromatography includes extracting by high-speed counter-current chromatography and purifying twice to obtain high-purity product. Its advantages are high purity (98%), and high output rate, and saving solvent.

Description

Technical field: [0001] The invention relates to a method for separating and preparing high-purity salidroside from natural plant rhodiola rosea. Background technique: [0002] The genus Rhodiola (Rhodiola L.) of the sedum family is a perennial herb or subshrub plant. There are more than 90 species of Rhodiola in the world, and there are nearly 80 species in my country, most of which are born at an altitude of 3500 to 5000 meters. On limestone, granite, mountain streams or valley rocks. Rhodiola rosea is used as medicine with the whole herb, which has the effects of clearing the lung and relieving cough, hemostasis and bandage. In ancient times, it was also used as a tonic and strong medicine. In recent years, it has been found that Rhodiola not only has the nourishing and strengthening effects of ginseng and Acanthopanax, but also is superior to these two drugs in some aspects. No side effects mentioned above. In accordance with the "Food Safety Toxicology Evaluation Pro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H1/08C07H15/18
Inventor 韩笑张天佑
Owner 北京天纯维通生物技术有限公司
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