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Method for measuring dissolution rate of obeticholic acid tablets

A technology of obeticholic acid tablets and obeticholic acid, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of insufficient detection sensitivity, low content of dissolution samples of obeticholic acid tablets, etc., and achieve simple reaction conditions Ease of operation, high sensitivity, and strong specificity

Inactive Publication Date: 2018-05-25
NCPC NEW DRUG RES & DEV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] 1 The object of the present invention is to provide a detection method for the dissolution rate of obeticholic acid tablets, aiming to solve the problems of low sample content and insufficient detection sensitivity of obeticholic acid tablets. The detection method is sensitive, accurate, reliable and reproducible. good sex

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  • Method for measuring dissolution rate of obeticholic acid tablets
  • Method for measuring dissolution rate of obeticholic acid tablets
  • Method for measuring dissolution rate of obeticholic acid tablets

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Example 1 Methodology Validation of Dissolution Detection of Obeticholic Acid Tablets

[0048] 1 Selection of measurement wavelength

[0049] Instruments and reagents: Waters 2695 liquid chromatograph, Tianda Tianfa RCZ-8m dissolution tester, aglent phenyl chromatography column (4.6*250mm, 5μm); acetonitrile-methanol is chromatographically pure, water is ultrapure water, other reagents For analytical purity.

[0050] Prepare the test solution, use the excitation wavelength of 420nm to scan the absorption wavelength of 440 nm to get the maximum value, then use the obtained value to return to scan the excitation wavelength, and then use the newly obtained excitation wavelength to scan the absorption wavelength to obtain a suitable detection wavelength range: The excitation wavelength is 384nm~404nm, the emission wavelength is 421nm~440nm, and the most sensitive wavelength: the excitation wavelength is 384nm, and the emission wavelength is 421nm.

[0051] 2 Detection lim...

Embodiment 2

[0058] Example 2 Determination of the Dissolution Profile of Obeticholic Acid Tablets in Phosphate Buffered Saline

[0059] Step 1, solution preparation

[0060] Preparation of the test solution: Take 6 units of obeticholic acid tablets (specification 5 μg), use the second method device of the dissolution method (Chinese Pharmacopoeia 2015 edition four), use pH 6.8 phosphate buffer 900ml as the dissolution medium , the rotating speed is 50 revolutions per minute, operate according to the law, take 5ml of the solution at 5 minutes, 10 minutes, 15 minutes, 30 minutes, 45 minutes, 60 minutes, 90 minutes, and 120 minutes, filter, and accurately measure the continued filtrate as the supply Test solution.

[0061] Preparation of the reference substance solution: Precisely measure the appropriate amount of the reference substance, add the corresponding dissolution medium to make solutions containing 1 μg, 2 μg, 5 μg, 7 μg, and 10 μg of obeticholic acid in each 1 ml respectively as a...

Embodiment 3

[0085] Example three: Determination of the dissolution rate of obeticholic acid tablets in water

[0086] 1 solution preparation

[0087] Preparation of the test solution: Take 6 units of obeticholic acid tablets, use the second method device of the dissolution method (Chinese Pharmacopoeia 2015 edition four), use 900ml water as the dissolution medium, and the speed is 50 rpm, and operate according to the law , get solution 5ml respectively in 5 minutes, 10 minutes, 15 minutes, 30 minutes, 45 minutes, 60 minutes, 90 minutes, 120 minutes, filter, and precision measures continued filtrate as need testing solution.

[0088] 2 Preparation of the reference substance solution: Accurately measure an appropriate amount of the reference substance, add the corresponding dissolution medium to make a solution containing about 3 micrograms of obeticholic acid per 1 ml as the reference substance solution.

[0089] 3 Extraction and evaporation: Accurately measure 5ml of the test solution an...

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Abstract

The invention discloses a method for measuring the dissolution rate of obeticholic acid tablets. The detection method comprises the following steps of (1) preparing solution; (2) extracting dry obeticholic acid; (3) carrying out derivatization reaction; (4) detecting by using high-performance liquid chromatography-fluorescence detector; (5) calculating to obtain the content of the obeticholic acidin a sample to be measured. According to the method disclosed by the invention, high-performance liquid chromatography measurement parameters and testing steps are reasonably selected, the fluorescence detector is selected, and an external standard method is adopted for quantification to realize the precise measurement of the dissolution rate of the obeticholic acid tablets. The method has the characteristics of economic and effective effects, strong specificity, high precision, strong interference resistance and high sensitivity.

Description

technical field [0001] The invention belongs to the field of drug detection and analysis, in particular to a method for detecting the dissolution rate of obeticholic acid tablets. Background technique [0002] Obeticholic acid tablet is a new member of the cholic acid family. It is small in size and difficult to test its dissolution rate. However, the dissolution of obeticholic acid and impurities is highly correlated with its in vivo effects, and the dissolution rate can be used for bioavailability control. Therefore, the detection and analysis of the dissolution rate of obeticholic acid tablets has important practical significance. However, studies have shown that the dissolution of obeticholic acid tablets cannot be detected by HPLC-UV, the detection sensitivity of differential refractometry is low, and the detection cost of HPLC-MS / MS is high. One of the important research directions is to choose appropriate derivatization reagents and simple pretreatment methods, and t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/884
Inventor 郭洪茹耿文飞左明昊徐彦孙莉张丽霞赵晶晶王芹芳李亚楠郭建鹏
Owner NCPC NEW DRUG RES & DEV
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