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

Method for Determination of Aniline Genotoxic Impurities in Solide Sodium Succinate New API

A technology of Solidium Sodium and raw materials, which is applied in the field of drug detection of Solidium Succinate New Raw Materials, to achieve the effects of reducing environmental hazards, high precision and good accuracy

Active Publication Date: 2020-09-29
上海明捷医药科技有限公司
View PDF3 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to solve the existing 4-chloroaniline and (-)-4'-chloroaniline tartaric acid content determination problem that there is no quality standard to check, and to provide a method for the determination of aniline in the new raw material drug of solidium succinate The method of genotoxic impurities has the advantages of short detection time, good accuracy, high precision and good repeatability

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 Determination of Aniline Genotoxic Impurities in Solide Sodium Succinate New API
  • Method for Determination of Aniline Genotoxic Impurities in Solide Sodium Succinate New API
  • Method for Determination of Aniline Genotoxic Impurities in Solide Sodium Succinate New API

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] A method for the determination of genotoxic impurities in a new raw material drug of sodium succinate, including the following steps:

[0041] S1. Prepare 4-chloroaniline and (-)-4'-chloroaniline wine with 4-chloroaniline and (-)-4'-chloroaniline tartaramic acid as the reference substance and 50% acetonitrile aqueous solution as the solvent Paraffinic acid reference substance solution, take the new sodium succinate raw material drug, and dissolve it with 50% acetonitrile aqueous solution to obtain the test solution;

[0042] S2. Prepare two 4-chloroaniline and (-)-4'-chloroaniline tartaramic acid reference solutions in parallel, and obtain 4-chloroaniline and (-)- in the reference solution by UPLC-MS method. 4'-Chloroaniline tartaric acid peak area, calculate the ratio of the peak area to the concentration of the reference solution to obtain the response factors of 4-chloroaniline and (-)-4'-chloroaniline tartaric acid;

[0043] S3. Take the test solution and detect it by UPL...

Embodiment 2

[0058] The linear range of the measurement method provided in Example 1 was investigated.

[0059] Take 10mg of 4-chloroaniline and (-)-4'-chloroaniline tartaramic acid in a 10mL volumetric flask, dissolve and dilute to the mark with 50% acetonitrile, shake well, as the reference substance stock solution 1; accurately measure Put 300μL of reference substance stock solution 1 in a 100mL volumetric flask, dilute to the mark with 50% acetonitrile, shake well, and serve as reference substance stock solution 2;

[0060] Pipette 0.05mL, 0.25mL, 0.4mL, 0.5mL, 0.75mL, 1mL of the reference substance stock solution 2 respectively into a 10mL volumetric flask, dilute to the mark with 50% acetonitrile, shake well, and mark them as L-10 , L-50, L-80, L-100, L-150 and L-200. Pipette 0.1 mL of L-100 into a 10 mL volumetric flask, dilute to the mark with 50% acetonitrile, and shake up to make L-1%.

[0061] According to the measurement method provided in Example 1, samples were injected and determ...

Embodiment 3

[0065] The standard addition recovery test of the determination method provided in Example 1.

[0066] The accuracy of the measurement method provided in Example 1 was analyzed by the method of standard addition and recovery.

[0067] Take 10 mg of the new raw material of solitary sodium succinate, accurately weigh it, and place 11 parts in parallel in a 10 mL volumetric flask. Take 2 parts of them and dissolve them with 50% acetonitrile to the mark, mix well, and determine 4 in the sample. -Chloroaniline and (-)-4'-Chloroaniline tartaramic acid content; take 3 of them, add 0.25mL reference substance stock solution 2, dissolve it with 50% acetonitrile to the mark, and mix well, as 50% Add standard recovery solution; take 3 of them, add 0.5mL reference substance stock solution 2, dissolve to the mark with 50% acetonitrile, mix well, as a 100% standard recovery solution; take 3 of them, add 0.7 mL of reference substance stock solution 2, dissolve it with 50% acetonitrile to the mark...

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
volume ratioaaaaaaaaaa
volume ratioaaaaaaaaaa
volume ratioaaaaaaaaaa
Login to View More

Abstract

The invention provides a method for determining aniline-type genotoxic impurities in a novel solifenacin succinate crude drug. The method comprises the steps that 4-chloroaniline and (-)-4'-chloroaniline tartramide acid are used as reference substances, a 50% of acetonitrile water solution is used as a solvent, reference substance solutions of the 4-chloroaniline and the (-)-4'-chloroaniline tartramide acid are prepared, the novel solifenacin succinate crude drug is obtain and is dissolved with 50% of acetonitrile water solution to obtain a test solution; detection is performed with a UPLC-MSmethod, the peak areas of the 4-chloroaniline and the (-)-4'-chloroaniline tartramide acid in the reference substance solutions are respectively obtained, and respective response factors are calculated; the test solution is detected by the UPLC-MS method, the peak area of the test solution is obtained, and the content of the 4-chloroaniline and the (-)-4'-chloroaniline tartramide acid in the testsolution is calculated according to the response factors. The method has the advantgaes of being short in detection time, good in accuracy, high in precision and good in repeatability.

Description

Technical field [0001] The invention belongs to the technical field of drug detection for a new sodium succinate raw material drug, and specifically relates to a method for determining aniline genotoxic impurities in a new sodium succinate raw material drug. Background technique [0002] 4-Chloroaniline and (-)-4'-Chloroaniline Tartaramic acid are aniline-type genotoxic impurities. They are widely used as starting materials and intermediates for drug synthesis. However, because 4-chloroaniline and (-) -4'-Chloroaniline Tartaramic acid is potentially toxic to cells, so it is necessary to control its content in the drug, but there is currently no quality standard for 4-chloroaniline and (-)-4'-chloroaniline tartaramide Method for determination of acid content. [0003] Therefore, there is an urgent need for a method with short detection time, good accuracy, high precision and good repeatability for the determination of aniline genotoxic impurities in the new raw material of solitary...

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 Patents(China)
IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/045G01N2030/8827
Inventor 嵇慧卿徐红兰顾凯朱子丰
Owner 上海明捷医药科技有限公司
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