Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Method for analyzing 6-ethylchenodeoxycholic acid and synthetic intermediate thereof by high-performance liquid chromatography

A high-performance liquid chromatography, obeticholic acid technology, applied in the field of high-performance liquid chromatography analysis of obeticholic acid and its synthetic intermediates, to achieve the effects of ensuring quality controllability, ensuring stability, and improving symmetry

Active Publication Date: 2018-04-17
JIANGSU SKYRUN PHARMA CO LTD
View PDF4 Cites 8 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no unified quality standard for obeticholic acid. In order to better control the quality of obeticholic acid raw materials, it is necessary to establish an effective separation and detection method

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
  • Method for analyzing 6-ethylchenodeoxycholic acid and synthetic intermediate thereof by high-performance liquid chromatography
  • Method for analyzing 6-ethylchenodeoxycholic acid and synthetic intermediate thereof by high-performance liquid chromatography
  • Method for analyzing 6-ethylchenodeoxycholic acid and synthetic intermediate thereof by high-performance liquid chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Instruments and Conditions:

[0027] High performance liquid chromatography: high performance liquid chromatography (Agilent 1260);

[0028] Chromatographic column: Thermo Syncronis C18 column (250mm×4.6mm, 5μm);

[0029] Mobile phase: 0.01mol / L potassium dihydrogen phosphate solution: acetonitrile:methanol=30:55:15(v:v:v);

[0030] Flow rate: 1.0ml / min;

[0031] Column temperature: 35°C;

[0032] Detector temperature: 35°C;

[0033] Injection volume: 100 μl.

[0034] Implementation steps:

[0035] Weigh 300 mg of obeticholic acid and 1 mg of each intermediate, respectively, and place in a 100 ml measuring bottle, dissolve with mobile phase, dilute to constant volume, and use it as the test solution. Measure 100 μl of the above solution and inject it into the liquid chromatograph, record the chromatogram, the result is as follows: figure 1 . Calculated by the area normalization method, the number of theoretical plates calculated by obeticholic acid is ≥2000, the...

Embodiment 2

[0038] Instruments and Conditions:

[0039] High performance liquid chromatography: high performance liquid chromatography (Agilent 1260);

[0040] Chromatographic column: Thermo Syncronis C18 column (250mm×4.6mm, 5μm);

[0041] Mobile phase: 0.005mol / L potassium dihydrogen phosphate solution: acetonitrile:methanol=30:55:15(v:v:v);

[0042] Flow rate: 1.0ml / min;

[0043] Column temperature: 35°C;

[0044] Detector temperature: 35°C;

[0045] Injection volume: 100 μl.

[0046] Implementation steps: Weigh 300 mg of obeticholic acid and 1 mg of each intermediate, put them in a 100 ml measuring bottle, dissolve with mobile phase, dilute to constant volume, and use it as the test solution. Measure 100 μl of the above solution and inject it into the liquid chromatograph, record the chromatogram, the result is as follows: figure 2 . Weigh 300mg of obeticholic acid synthesized independently and place it in a 100ml measuring bottle, dissolve it with mobile phase, dilute to cons...

Embodiment 3

[0050] Instruments and Conditions:

[0051] High performance liquid chromatography: high performance liquid chromatography (Agilent 1260);

[0052] Chromatographic column: Thermo Syncronis C18 column (250mm×4.6mm, 5μm);

[0053] Mobile phase: 0.005mol / L sodium dihydrogen phosphate solution: acetonitrile:methanol=25:57:18(v:v:v);

[0054] Flow rate: 1.0ml / min;

[0055] Column temperature: 40°C;

[0056] Detector temperature: 40°C;

[0057] Injection volume: 80 μl.

[0058] Implementation steps: Weigh 300 mg of obeticholic acid and 1 mg of each intermediate, put them in a 100 ml measuring bottle, dissolve with mobile phase, dilute to constant volume, and use it as the test solution. Measure 80 μl of the above solution and inject it into the liquid chromatograph, record the chromatogram, the result is as follows: Figure 4 . Weigh 300mg of obeticholic acid synthesized independently and place it in a 100ml measuring bottle, dissolve it with mobile phase, dilute to constant ...

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
concentrationaaaaaaaaaa
Login to View More

Abstract

The invention belongs to the technical field of pharmaceutical analysis and relates to a method for analyzing 6-ethylchenodeoxycholic acid and a synthetic intermediate thereof by high-performance liquid chromatography. The separation and detection method provided by the invention adopts an octadecyl silane bonded silica gel packed column with the chromatographic column temperature of 35-40 DEG C and a differential detector, and a phosphate buffer solution and an acetonitrile and methanol mixed solution are used for elution. The method provided by the invention realizes simple, quick and accurate separation and detection of the 6-ethylchenodeoxycholic acid and the synthetic intermediate thereof, and solves the problem of separation and detection of 6-ethylchenodeoxycholic acid-containing raw materials and preparations, thereby ensuring the quality controllability of the 6-ethylchenodeoxycholic acid and the 6-ethylchenodeoxycholic acid-containing compositions or preparations.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, and relates to a method for analyzing obeticholic acid and its synthetic intermediate by high performance liquid chromatography. Background technique [0002] Obeticholic acid is a farnesoid X receptor agonist, which indirectly inhibits the gene expression of cytochrome 7A1 (CYP7A1) by activating farnesoid X receptor. Since CYP7A1 is the rate-limiting enzyme of bile acid biosynthesis, obeticholic acid can inhibit bile acid synthesis for the treatment of primary biliary cirrhosis and nonalcoholic fatty liver disease. Obeticholic acid was successfully developed by Intercept Pharmaceuticals, Inc. in the United States. In May 2014, the US FDA granted Intercept Pharmaceuticals a fast track approval for obeticholic acid. Obeticholic acid is the first drug developed for the treatment of cholestatic liver disease in the past 20 years, and it is also the second drug approved by the FDA for the trea...

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): G01N30/02
CPCG01N30/02
Inventor 燕立波金永华姜向敏
Owner JIANGSU SKYRUN PHARMA CO LTD
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com