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Method for separating high-purity lactone type lovastatin from fermentum rubrum powder

A lovastatin, high-purity technology, applied in the field of extraction, separation and purification of effective substances, can solve the problems of high production cost, loss of lovastatin, waste of water and alcohol, etc. Simple process effect

Active Publication Date: 2015-10-07
LANZHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process is not only complicated, but also the ultrafiltration membrane is expensive and costly; the macroporous resin is fully adsorbed for the first time, and when it is detected that the effluent has lovastatin coming out, stop passing through the column, and some lovastatin will be lost. There is no guarantee that lovastatin will be completely adsorbed, and some lovastatin will be lost by desorbing impurities with distilled water for the second time; finally, desorbing lovastatin adsorbed on the resin with 45% ethanol solution is complicated, long and time-consuming. It is not easy to control the degree of elution, waste water and alcohol, the loss of lovastatin is large, the yield is low, the production cost is high, and it is not conducive to industrial production

Method used

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  • Method for separating high-purity lactone type lovastatin from fermentum rubrum powder
  • Method for separating high-purity lactone type lovastatin from fermentum rubrum powder
  • Method for separating high-purity lactone type lovastatin from fermentum rubrum powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] (1) Preparation of crude extract of Lovastatin

[0036] Add commercially available red yeast rice powder (purchased from Zhejiang Sanhe Biological Engineering Co., Ltd., batch number 2014012301, lovastatin content of 30.658mg / g) and 100% pure ethanol in a ratio of 10g / 500mL into a 1000mL round bottom flask. , Adjust the temperature of the heating device to 75℃, start timing when refluxing, reflux extraction for 5h, remove the reflux device, and use the suction filter device to filter while the vacuum pump pressure is 0.08Mpa to obtain the filtrate and the residue. The filtrate is pumped into the vacuum to concentrate The device is concentrated to obtain the crude extract of lovastatin; the ethanol in the filtrate is recovered and reused, and the filter residue is rich in polysaccharides, proteins, etc., which can be recovered as additives for animal feed.

[0037] (2) Separation of monomer lactone lovastatin

[0038] The crude extract of lovastatin obtained in step (1) and co...

Embodiment 2

[0041] (1) Preparation of crude extract of Lovastatin

[0042] The ethanol solution uses 95% ethanol by volume, the ratio of red yeast rice powder to ethanol solution is 10g / 250mL, the reflux temperature is 80°C, and the time is 4 hours; the vacuum pump pressure during suction filtration is 0.07Mpa, and the others are the same as in Example 1.

[0043] (2) Separation of monomeric lactone lovastatin:

[0044] The column chromatography silica gel is 100~200 mesh, the mass ratio of lovastatin crude extract and column chromatography silica gel is 1g: 2g, and the sample is mixed with 24g column chromatography silica gel. The mobile phase petroleum ether and ethyl acetate volume ratio It is 1:2, the flow rate is 4mL / min, and every 2mL is a fraction. When the mobile phase elutes to the first red band, the elution is stopped. Others are the same as in Example 1. 290 mg of feathery white lactone lovastatin crystals with higher purity were obtained, and the extraction rate was 94.6%.

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Abstract

The present invention discloses a new method for separating lactone type lovastatin from fermentum rubrum. According to the method, commercially available functional fermentum rubrum powder is adopted as a raw material, ethanol extraction and vacuum suction filtration are performed, silica gel column chromatography one-step separation is performed, and purity analysis and structure identification are performed respectively through a chromatography method and a spectroscopy method after concentration crystallization so as to obtain the lovastatin crystal having the purity of more than or equal to 98% and having the lactone type structure, wherein the extraction rate is more than or equal to 85%. According to the present invention, the method has characteristics of simple production equipment, simple and feasible process, simple operation, short time consuming, high bulk drug utilization rate and low production cost, and is the energy-saving and environmental protection method.

Description

technical field [0001] [The present invention relates to a new method for separating lactone-type lovastatin from red yeast rice powder, in particular to a method for separating high-purity lactone-type lovastatin by using column chromatography on silica gel, and belongs to the field of extraction, separation and purification of effective substances. Background technique [0002] Lovastatin is a common drug for treating hyperlipidemia. It was first discovered and isolated from Chinese red yeast rice powder by Japanese biochemist Endō Akira around 1976. It is a hydroxymethylglutaryl-CoA reductase (HMGR) inhibitor, which can inhibit the synthesis of cholesterol at the root. In the 1980s, it became a new type of blood lipid-regulating drug. Its trade names were Mingweixin, Luote, Xinlu, etc. It has unique curative effect and is known as a milestone in the treatment of cardiovascular system diseases. Mixed hyperlipidemia. At present, statins synthesized with lovastatin or its ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D309/30
CPCC07D309/30
Inventor 倪京满缑三虎王一杰
Owner LANZHOU UNIVERSITY
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