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

Detection method for 1-(2, 3-dichlorophenyl) piperazine hydrochloride and related substances thereof

A detection method, the technology of dichlorophenyl, applied in the field of detection, can solve the problems of affecting the purity of aripiprazole, the inability to detect effectively, the increase of related substances, etc., and achieve high sensitivity, short peak time and good separation Effect

Active Publication Date: 2020-02-28
四川弘远药业有限公司
View PDF6 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] And it is difficult to be removed in the post-treatment and refining process of aripiprazole, which increases the related substances in aripiprazole and greatly affects the purity of aripiprazole
[0008] In order to reduce the occurrence of side reactions, improve the yield and purity of aripiprazole, and avoid the follow-up complicated separation and purification process, it is necessary to carry out quality control on the raw material of 1-(2,3-dichlorophenyl)piperazine hydrochloride, However, the prior art does not disclose a detection method for related substances of 1-(2,3-dichlorophenyl)piperazine hydrochloride
The present invention measures aripiprazole and related substances in aripiprazole tablets by RP-HPLC methods such as Yu Hui [Journal of Southeast University (Medical Edition) March 2005, 24 (2)], Methodological research on the separation of related substances of aripiprazole by Zha Jianpeng et al. [Chinese Journal of Pharmaceutical Sciences, Volume 40, No. 2, January 2005], preparation and quality evaluation of aripiprazole oral film by Zhang Yuni et al. [China Pharmaceutical Industry Journal 2015, 46 (3)] etc. disclosed aripiprazole related substance detection method for detection of 1-(2,3-dichlorophenyl)piperazine hydrochloride related substance discovery, the existing aripiprazole 1-(2,3-dichlorophenyl)piperazine hydrochloride related substances cannot be effectively detected by the detection method of azole related substances

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
  • Detection method for 1-(2, 3-dichlorophenyl) piperazine hydrochloride and related substances thereof
  • Detection method for 1-(2, 3-dichlorophenyl) piperazine hydrochloride and related substances thereof
  • Detection method for 1-(2, 3-dichlorophenyl) piperazine hydrochloride and related substances thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0122] 1. Sample preparation

[0123] Preparation of sample solution: take an appropriate amount of 1-(2,3-dichlorophenyl)piperazine hydrochloride sample, add acetonitrile to make a 0.4mg / ml solution of the test solution;

[0124] Preparation of reference solution: take 2,3-dichloroaniline, 1-(2-chlorophenyl)piperazine hydrochloride, 1-(3-chlorophenyl)piperazine hydrochloride, 1-(2,3 -Chlorophenyl)piperazine dimer hydrochloric acid reference substance in appropriate amount, accurately weighed, add acetonitrile to make 0.4μg of 2,3-dichloroaniline, 1-(2-chlorophenyl)piperazine hydrochloride per 1ml A mixed solution of 0.4 μg, 0.4 μg of 1-(3-chlorophenyl)piperazine hydrochloride, and 0.4 μg of 1-(2,3-chlorophenyl)piperazine dimer hydrochloride is obtained;

[0125] 2. Detection

[0126] time (min) Mobile phase A (%) Mobile phase B (%) 0 85 15 10 70 30 25 15 85 25.1 85 15 30 85 15

[0127] name Quantitation limit (ug / m...

Embodiment 2

[0129] 1. Sample preparation

[0130] Test sample solution preparation: Example 1

[0131] Preparation of reference solution: Example 1

[0132] 2. Detection

[0133] time (min) Mobile phase A (%) Mobile phase B (%) 0 85 15 10 70 30 25 15 85 25.1 85 15 30 85 15

[0134] name Quantitation limit (ug / ml) Detection limit (ug / ml) degree of separation Impurity 1 0.04 0.01 6.46 14954 Impurity 2 0.01ug / ml 0.003ug / ml 7.43 27558 main ingredient 0.04ug / ml 0.013ug / ml 21.53 5529 Impurity 3 0.02ug / ml 0.005ug / ml 23.73 378133 Impurity 4 0.04ug / ml 0.01ug / ml —— 83449

Embodiment 3

[0136] 1. Sample preparation

[0137] Test sample solution preparation: Example 1

[0138] Preparation of reference solution: Example 1

[0139] 2. Detection

[0140] time (min) Mobile phase A (%) Mobile phase B (%) 0 85 15 10 70 30 25 15 85 25.1 85 15 30 85 15

[0141] name Quantitation limit (ug / ml) Detection limit (ug / ml) degree of separation Number of theoretical plates Impurity 1 0.04ug / ml 0.01ug / ml 6.49 15422 Impurity 2 0.01ug / ml 0.003ug / ml 7.35 29029 main ingredient 0.04ug / ml 0.013ug / ml 20.28 5739 Impurity 3 0.03ug / ml 0.01ug / ml 9.25 395840 Impurity 4 0.04ug / ml 0.01ug / ml —— 26697

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

No PUM Login to View More

Abstract

The invention provides a detection method for 1-(2, 3-dichlorophenyl) piperazine hydrochloride and related substances thereof. According to liquid chromatography detection conditions of the method, octadecylsilane chemically bonded silica is used as a chromatographic column of a filler, an acetonitrile-disodium hydrogen phosphate buffer solution serves as the mobile phase A, acetonitrile-phosphoric acid serves as the mobile phase B, the detection wavelength is 254nm, and elution is performed in a gradient manner. The method is rapid, efficient, stable and accurately, and can be used to rapidlyand effectively related substances of 1-(2, 3-dichlorophenyl) piperazine hydrochloride.

Description

technical field [0001] The invention relates to a detection method, in particular to a high-performance liquid chromatography detection method of 1-(2,3-dichlorophenyl)piperazine hydrochloride and related substances. Background technique [0002] 1-(2,3-Dichlorophenyl)piperazine hydrochloride, also known as 1-(2,3-dichlorophenyl)-piperazine monohydrochloride, 2,3-dichlorophenylpiperazine Monohydrochloride is a commonly used pharmaceutical intermediate, and its structural formula is as follows: [0003] [0004] Molecular formula: C 10 H 13 C l3 N 2 , molecular weight: 267.58. [0005] 1-(2,3-Dichlorophenyl)piperazine hydrochloride is the intermediate of phenylpiperazine antidepressants, especially the key starting material for the synthesis of neuroregulatory drug aripiprazole. According to literature reports: At present, 1-(2,3-dichlorophenyl)piperazine hydrochloride is mainly synthesized by using 2,3-dichloroaniline as 1-(2,3-dichlorophenyl)piperazine hydrochlorid...

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
IPC IPC(8): G01N30/34G01N30/02
CPCG01N30/34G01N30/02
Inventor 柯潇范贵勤张良郑军严峻
Owner 四川弘远药业有限公司
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