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A kind of high performance liquid chromatography analysis method of obeticholic acid

A technology of high performance liquid chromatography and obeticholic acid, which is applied in the field of drug analysis and detection, can solve the problems of no uniform quality standard for obeticholic acid, and achieve the effects of weak ultraviolet absorption, high theoretical plate number and high detection sensitivity

Active Publication Date: 2021-07-13
LIVZON NEW NORTH RIVER PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] At present, there is no unified quality standard for obeticholic acid. In order to ensure the quality of subsequent research and production of obeticholic acid, quality control of obeticholic acid raw materials is required

Method used

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  • A kind of high performance liquid chromatography analysis method of obeticholic acid
  • A kind of high performance liquid chromatography analysis method of obeticholic acid
  • A kind of high performance liquid chromatography analysis method of obeticholic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] High performance liquid chromatography analysis method of obeticholic acid

[0038] Instruments and conditions:

[0039] High performance liquid chromatography: Ultimate 3000 (Thermo Fisher);

[0040] Electrospray detector atomization temperature: 40°C;

[0041] Chromatographic column: C18, specification 4.6*150mm, 3.5μm;

[0042] Mobile phase; mobile phase A: acetonitrile, mobile phase B: methanol, mobile phase C: formic acid aqueous solution (pH=3.5);

[0043] Gradient elution program:

[0044] time (min) Mobile phase A(%) Mobile phase B(%) Mobile phase C(%) 0.0 48 0 52 15.0 48 20 32 45.0 90 0 10 50.0 48 0 52

[0045] Flow rate: 1.0mL / min;

[0046] Column temperature: 40°C;

[0047] Injection volume: 20 μL.

[0048] Solution preparation:

[0049] Preparation of formic acid aqueous solution: Measure 1000 mL of distilled water, add formic acid dropwise, and adjust the pH to 3.5.

[0050] Preparation of the test sol...

Embodiment 2

[0053] High performance liquid chromatography analysis method of obeticholic acid

[0054] Other experimental conditions are the same as in Example 1, only mobile phase C: acetic acid aqueous solution is different.

[0055] Preparation of acetic acid aqueous solution: Measure 1000 mL of distilled water, add acetic acid dropwise, and adjust the pH to 3.5

[0056] Depend on figure 2 It can be seen that the retention time of obeticholic acid is 21.402min, the tailing factor is 0.99, the peak shape is good, and the number of theoretical plates is 32630.

[0057] System Adaptability Experiment Results

[0058] System Suitability Test for Determination of Obeticholic Acid

[0059] Instruments and conditions:

[0060] High performance liquid chromatography: Ultimate 3000 (Thermo Fisher);

[0061] Electrospray detector: atomization temperature 40°C;

[0062] Chromatographic column: C18, specification 4.6*150mm, 3.5μm;

[0063] Mobile phase; mobile phase A: acetonitrile, mobile...

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Abstract

The invention discloses a high-performance liquid chromatography analysis method of obeticholic acid, which is detected by reverse-phase high-performance liquid chromatography using an electrospray detector (CAD), comprising the following steps: a, preparing a test solution; b , adopt the reversed-phase high-performance liquid chromatography of charged spray detector (CAD) to detect need testing solution; Wherein elution adopts gradient mode elution, mobile phase A is acetonitrile, mobile phase B is methyl alcohol, and mobile phase C is formic acid Any one of aqueous solution or acetic acid aqueous solution. The high-efficiency liquid phase analysis method of obeticholic acid provided by the invention adopts an electrospray detector (CAD), has high detection sensitivity, has the advantages of simplicity, accuracy, reliability, and high theoretical plate number, and can effectively detect obeticholic acid content.

Description

technical field [0001] The invention belongs to the field of drug analysis and detection, and relates to a high performance liquid chromatography analysis method of obeticholic acid. 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. Its structural formula is [0003] [0004] Obeticholic acid was successfully developed by Intercept Pharmaceutical Company of the United States. It is the first drug developed for the treatment of cholestatic liver disease in two decades. The study was performed in patients who did not respond adequately to or could not tolerate the older standard of care, ursodeoxycholic acid. Obeticholic acid (OCA) in...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/89
CPCG01N30/89
Inventor 陈月嫦谢伟健姜桥王标李冰冰王龙书
Owner LIVZON NEW NORTH RIVER PHARMA