Unlock instant, AI-driven research and patent intelligence for your innovation.

Analysis method of preparation process of statin compound

An analysis method and technology of preparation process, applied in the field of preparation of statin compounds, can solve the problems of difficult analysis, large interference, rough estimation, etc., and achieve the effect of shortening analysis time, eliminating interference factors, and changing operation steps

Inactive Publication Date: 2017-04-19
PEKING UNIV FOUNDER GRP CO LTD +2
View PDF3 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] 1. TLC thin-layer chromatography method, using TLC thin-layer chromatography plate can only make a rough estimate, using thin-layer chromatography method has low sensitivity and does not meet the advanced nature of production indicators;
[0006] 2. The detection method of high performance liquid chromatography adopts a UV detector and uses methanol as the mobile phase. The detection wavelength is 238nm (absorption wavelength). The short wavelength has large interference and is easily affected by mobile phase and sample processing methods. It brings certain difficulties, and the sample determination time is long, the selectivity is relatively poor, and it is difficult to detect products with similar structures

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Analysis method of preparation process of statin compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Example 1: Selection of chromatographic conditions

[0047] 1.1 Selection of mobile phase

[0048] The reason why acetonitrile and water are selected as the mobile phase in the present invention is based on the consideration of the following factors: eliminate the interference factors of the mobile phase detection during the determination to improve the reliability and accuracy; improve the separation between the peaks; and use gradient washing Monacolin J acid (Monacolin J acid), α-dimethylbutyryl-S-methyl propionate (DMB-S-MMP), lovastatin sodium, simvastatin ammonium salt, lovastatin , Simvastatin achieves baseline effective separation.

[0049] 1.2 Selection of detection wavelength

[0050] Detection is performed at a wavelength of 238nm.

[0051] 1.3 Sample solution preparation

[0052] Accurately weigh an appropriate amount of the test substance, add an appropriate amount of methanol to dissolve and dilute to the mark, and shake it up to obtain a test solution of about 800...

Embodiment 2

[0055] Example 2: Determination of standard repeatability

[0056] Take the mixed standard solution and inject 10μL, continuously inject 6 needles, calculate the RDS% based on the peak area. The results are shown in Table 2.

[0057] Table 2 Repeatability

[0058]

Embodiment 3

[0060] Monacrine J acid is obtained by enzymatic hydrolysis of lovastatin sodium by sampling and testing regularly.

[0061] Test product: Determination of 80h fermentation product during fermentation conversion production stage:

[0062] Precisely weigh about 0.1g of the test product in a 10mL volumetric flask, dissolve it with methanol, sonicate for 7min, constant volume, shake up, and filter with an organic 0.22μm filter membrane to obtain the test solution. Injection volume: 10μL. Nacrine J acid is more than 99%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
wavelengthaaaaaaaaaa
injection volumeaaaaaaaaaa
Login to View More

Abstract

The invention provides an analysis method of a preparation process of a statin compound. Reversed phase high-performance liquid chromatography is adopted in component analysis of a mixture containing Monacolin Jacid, alpha-dimethylbutyryl-S-methyl mercaptopropionate, lovastatin sodium salt, simvastatin ammonium salt, lovastatin and / or simvastatin; gradient elution is adopted; a buffer salt solution and acetonitrile are taken as a mobile phase A and a mobile phase B respectively. The analysis method can be used for analysis of related compounds in production process, influence factors are eliminated, analysis time is shortened greatly, operation is simple, reliable, and accurate, and effective means are provided for statin compound preparation process research and production process industrialized management.

Description

Technical field [0001] The invention relates to the field of preparation of statin compounds, in particular to an analysis method for the preparation process of statin compounds and its application in enzyme conversion and synthetic production of statin compounds. Background technique [0002] Simvastatin is a semi-synthetic derivative of lovastatin. The traditional production process uses lovastatin as a raw material to obtain simvastatin through chemical synthesis. Now it can be produced by fermentation method. Firstly, lovastatin is opened under the action of alkali to obtain lovastatin sodium, and then monacrine J acid is obtained by enzymatic hydrolysis, and then α-disulfide is simultaneously added by acylation enzyme method. The side chain of methyl butyryl-S-propionic acid methyl ester (DMB-S-MMP) gives simvastatin ammonium salt, and finally the ammonia is removed by refluxing toluene to obtain simvastatin. The process is environmentally friendly and has few by-products, ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
CPCG01N30/88
Inventor 岳光张洪兰谢云
Owner PEKING UNIV FOUNDER GRP CO LTD