Detection method of genotoxic impurities in vilazodone hydrochloride

A technology of vilazodone hydrochloride and a detection method is applied in the field of detection of genotoxic impurity diamine and its hydrochloride in vilazodone hydrochloride, can solve the problems of difficulty in detection, low limit and the like, and achieves a good linear relationship, Realize the effect of effective control and high detection sensitivity

Active Publication Date: 2020-11-24
CSPC ZHONGQI PHARM TECH (SHIJIAZHUANG) CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to its low limit and difficult detection, there is no literature on the detection method of this genotoxic impurity

Method used

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  • Detection method of genotoxic impurities in vilazodone hydrochloride
  • Detection method of genotoxic impurities in vilazodone hydrochloride
  • Detection method of genotoxic impurities in vilazodone hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] The localization test of embodiment 1 two (2-chloroethyl) amine hydrochloride

[0042]Gas phase conditions: use a cross-linked polyethylene glycol capillary column (DB-Wax, 30m×0.25mm×0.25μm), column temperature: 50°C, keep for 2min; heat up to 100°C at 20°C / min, keep for 5min; Gas: high-purity helium, carrier gas flow rate: 1.0ml / min, sampling method: split injection, split ratio: 5:1; purge carrier gas: nitrogen, purge temperature: 20°C time: 11min flow rate: 40ml / min, desorption temperature: 250°C time: 2min flow rate: 300ml / min, baking temperature: 280°C time: 2min flow rate: 200ml / min.

[0043] Mass spectrometry conditions: ionization source is EI, ion source temperature: 230°C, analyzer: single quadrupole mass analyzer, monitoring mode is single ion detection mode (SIM).

[0044] Blank solution: 0.1mol / L NaOH solution.

[0045] Reference substance stock solution configuration: Take 3.75mg of bis(2-chloroethyl)amine hydrochloride reference substance, weigh it ac...

Embodiment 2

[0049] Embodiment 2 methodological investigation

[0050] Gas phase conditions: use a cross-linked polyethylene glycol capillary column (DB-Wax, 30m×0.25mm×0.25μm), column temperature: 50°C, keep for 2min; heat up to 100°C at 20°C / min, keep for 5min; Gas: high-purity helium, carrier gas flow rate: 1.0ml / min, sampling method: split injection, split ratio: 5:1; purge carrier gas: nitrogen, purge temperature: 20°C time: 11min flow rate: 40ml / min, desorption temperature: 250°C time: 2min flow rate: 300ml / min, baking temperature: 280°C time: 2min flow rate: 200ml / min. Mass spectrometry conditions: ionization source is EI, ion source temperature: 230°C, analyzer: single quadrupole mass analyzer, monitoring mode is single ion detection mode (SIM).

[0051] Reference substance solution: with reference to Example 1

[0052] 1. Linearity and range

[0053] Precisely measure 80 μl, 400 μl, 600 μl, 1.00ml, 1.60ml, 2ml of the stock solution of the reference substance solution, dissolve...

Embodiment 3

[0067] Example 3 Sample Determination

[0068] Gas phase conditions: use a cross-linked polyethylene glycol capillary column (DB-Wax, 30m×0.25mm×0.25μm), column temperature: 50°C, keep for 2min; heat up to 100°C at 20°C / min, keep for 5min; Gas: high-purity helium, carrier gas flow rate: 1.0ml / min, sampling method: split injection, split ratio: 5:1; purge carrier gas: nitrogen, purge temperature: 20°C time: 11min flow rate: 40ml / min, desorption temperature: 250°C time: 2min flow rate: 300ml / min, baking temperature: 280°C time: 2min flow rate: 200ml / min.

[0069] Mass spectrometry conditions: ionization source is EI, ion source temperature: 230°C, analyzer: single quadrupole mass analyzer, monitoring mode is single ion detection mode (SIM).

[0070] Solution preparation:

[0071] Please refer to Example 1 for the preparation of the reference solution.

[0072] Test solution: Accurately weigh 1 g of vilazodone hydrochloride, add 100 ml of 0.1 mol / L sodium hydroxide solution f...

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Abstract

The invention relates to a detection method for a genotoxic impurity bis(2-chloroethyl)amine and hydrochloride thereof in vilazodone hydrochloride. According to the method, gas chromatography-mass spectrometry is employed for determination; a cross-linked polyethylene glycol capillary chromatographic column is used in gas chromatography; and an electron bombardment ionization source is employed for mass spectrometry. The detection method has high sensitivity, high accuracy and good durability, can effectively control the mass of the genotoxic impurity bis(2-chloroethyl)amine and hydrochloridethereof in vilazodone hydrochloride, reduces side reactions in medication of patients and guarantees the medication security of patients to a certain degree.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a method for detecting genotoxic impurity bis(2-chloroethyl)amine and its hydrochloride in vilazodone hydrochloride. Background technique [0002] Vilazodone hydrochloride (Vilazodone) is a dual-action selective 5-HT reuptake inhibitor and 5-HT1A receptor partial agonist developed by Trovis Pharmaceuticals LLC of the United States, and was approved in January 2011. The U.S. Food and Drug Administration has approved the marketing, and the trade name is Viibryd, which is used for the treatment of severe depression in adults. Its structural formula is as follows: [0003] [0004] For the synthesis process of vilazodone hydrochloride, literature (TIMO H, HENNING B, ROLF G, et al.Synthesis and structure-activity relationship in a class of indolebutylpiperacines as dual5-HT1A receptor agonists and sero toninreuptake inhibitors[J].J Med Chem , 2004,47(19):4684-4692.) d...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 张倩如张红芬郭文敏张琪杨占坤
Owner CSPC ZHONGQI PHARM TECH (SHIJIAZHUANG) CO LTD
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