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Method for measuring robenidine hydrochloride and metabolite residues in aquatic product through high performance liquid chromatography-tandem mass spectrometry

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

Active Publication Date: 2019-05-03
武汉言必行科技股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • Method for measuring robenidine hydrochloride and metabolite residues in aquatic product through high performance liquid chromatography-tandem mass spectrometry
  • Method for measuring robenidine hydrochloride and metabolite residues in aquatic product through high performance liquid chromatography-tandem mass spectrometry
  • Method for measuring robenidine hydrochloride and metabolite residues in aquatic product through 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 measuring robenidine hydrochloride and metabolite residues in an aquatic product through high performance liquid chromatography-tandem mass spectrometry based on atime segment technology. The method comprises: A, weighing aquatic product muscle tissues, adding acetonitrile with 1% formic acid, anhydrous magnesium sulfate, and ODS, and extracting and purifying;B, using high performance liquid chromatography-tandem mass spectrometry to carry out positive and negative ion mode switching and detect the residues of robenidine hydrochloride, parachlorobenzoic acid and p-chlorobenzamide acetic acid in aquatic product muscles in different time periods; and C, carrying out standard curve method quantification: using an internal standard method to quantify therobenidine hydrochloride, taking robenidine hydrochloride-d8 as an internal standard, and using an external standard method to quantify the p-chlorobenzoyl aminoacetic acid and the parachlorobenzoic-acid. Operation is simple, a matrix effect is low, a detection limit is low and accuracy and precision are high.

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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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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