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A method for the determination of prohezidine hydrochloride and its metabolite residues in aquatic products by high performance liquid chromatography-tandem mass spectrometry

A technology of high performance liquid chromatography and prohexidine hydrochloride, applied in the direction of measuring devices, instruments, scientific instruments, etc., to achieve the effects of high accuracy and precision, low detection limit, and easy operation

Active Publication Date: 2021-09-24
武汉言必行科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, there are no reports or patent applications on the method for the determination of chlorhexidine hydrochloride and its metabolites p-chlorobenzoic acid and p-chlorobenzamide acetic acid residues in aquatic products by high performance liquid chromatography-tandem mass spectrometry

Method used

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  • A method for the determination of prohezidine hydrochloride and its metabolite residues in aquatic products by high performance liquid chromatography-tandem mass spectrometry
  • A method for the determination of prohezidine hydrochloride and its metabolite residues in aquatic products by high performance liquid chromatography-tandem mass spectrometry
  • A method for the determination of prohezidine hydrochloride and its metabolite residues in aquatic products by high performance liquid chromatography-tandem mass spectrometry

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Embodiment 1

[0026] Example 1 Method optimization for the determination of prohezidine hydrochloride and its metabolite residues in aquatic products by high performance liquid chromatography-tandem mass spectrometry

[0027] 1. Optimization of mass spectrometry conditions

[0028] Inject 10 mg / L of chlorhexenidine hydrochloride, chlorhexidine hydrochloride-d8, p-chlorobenzamide acetic acid, and p-chlorobenzoic acid into the mass spectrometer through a syringe pump, and the responses of the above-mentioned target substances in positive ion and negative ion modes The results showed that the responsivity of chlorhexidine hydrochloride and chlorhexidine-d8 in positive ion mode was 5 times and 3 times that in negative ion mode. However, the response values ​​of p-chlorobenzamide acetic acid and p-chlorobenzoic acid in the negative ion mode were 2 times and 1 times that in the positive ion mode. Therefore, chlorhexidine hydrochloride and chlorhexidine-d 8 The analysis was performed in positive...

Embodiment 2

[0037] A method for the determination of prohezidine hydrochloride and its metabolite residues in aquatic products based on high performance liquid chromatography-tandem mass spectrometry of time-segmented technology, the steps are:

[0038] A. Weigh 1g of homogeneous grass carp muscle sample in a 15mL centrifuge tube, add chlorhexenidine hydrochloride, p-chlorobenzamide acetic acid and p-chlorobenzoic acid standard solution to make chlorhexenidine hydrochloride, p-chlorobenzamide The concentrations of acetic acid and p-chlorobenzoic acid were 1, 3, 50, 100, 400 μg / kg, 2.5, 5, 50, 100, 400 μg / kg, 5, 10, 50, 50 μg / kg, and then 20 μL of 1 mg / kg L Chlorhexidine Hydrochloride-d 8 Internal standard solution, shake for 30s, add 5mL extractant acetonitrile containing 1% formic acid, shake for 30s, ultrasonically extract for 5min, add 1g of anhydrous magnesium sulfate to remove water and part of fat in the sample, vortex. Centrifuge at 8000r / min for 5min, put the upper liquid in anot...

Embodiment 3

[0056] Application of time-segmented high performance liquid chromatography-tandem mass spectrometry for the determination of prohezidine hydrochloride and its metabolite residues in aquatic products:

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Abstract

The invention discloses a method for determining the residual amount of chlorhexidine hydrochloride and its metabolites in aquatic products by high performance liquid chromatography-tandem mass spectrometry based on time-segmented technology. The steps are: A. Weigh the muscle tissue of aquatic products, add acetonitrile containing 1% formic acid, anhydrous magnesium sulfate, ODS extraction and purification; B. Use high performance liquid chromatography-tandem mass spectrometry to switch between positive and negative ion modes and detect chlorophenylguanidine hydrochloride, p-chlorobenzoic acid, and p-chlorobenzene in muscle of aquatic products in different time periods The residual amount of formamide acetic acid; C. Quantification by standard curve method: Chlorhexenidine hydrochloride adopts internal standard method to quantify, and Chlorhexenidine hydrochloride-d 8 As internal standard, p-chlorobenzamidoacetic acid and p-chlorobenzoic acid were quantified by external standard method. The method is easy to operate, has low matrix effect, low detection limit, high accuracy and precision.

Description

technical field [0001] The invention belongs to the technical field of safety detection of aquatic products, and in particular relates to a method for determining the residual amount of chlorhexidine hydrochloride and its metabolites in aquatic products by high-performance liquid chromatography-tandem mass spectrometry based on time-segmentation technology. Background technique [0002] Chlorhexenidine hydrochloride (1,3-bis(p-chlorobenzylidene amino)guanidine hydrochloride) belongs to guanidine derivatives and is a kind of achiral chemical synthesis drug. Chlorhexidine Hydrochloride-d 8 It is formed by replacing the 8 hydrogen atoms on the two benzene rings of chlorhexidine hydrochloride with heavy hydrogen atoms. Chlorhexidine hydrochloride is permitted in Europe as a feed additive to prevent coccidiosis in broilers, turkeys and rabbits. Chlorhexidine hydrochloride is used to treat fish sporozoiosis in my country. Studies have shown that preventive feeding of prohexidin...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/72
Inventor 刘永涛王桢月艾晓辉董靖胥宁杨秋红杨移斌周顺
Owner 武汉言必行科技股份有限公司
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