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Method for simultaneously measuring various drug residues in honey by utilizing liquid chromatogram tandem mass spectrum isotope dilution method

A technology of isotope dilution and tandem mass spectrometry is applied in the field of detection of various types of drug residues in honey, which can solve the problems of high detection cost, long detection period, multiple manpower and material resources, and achieve the effect of low detection cost and maintenance of food safety.

Inactive Publication Date: 2012-09-26
THE INSPECTION & QUARANTINE TECH CENT ZHEJIANG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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Problems solved by technology

[0005] With the improvement of people's food safety awareness, a batch of honey often needs to detect many types of drug residues. Therefore, according to the traditional analysis method, it needs a longer detection cycle, more manpower and material resources, and high detection cost, which cannot meet the requirements of current drugs. The variety is increasing and the demand for analysis throughput is increasing

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  • Method for simultaneously measuring various drug residues in honey by utilizing liquid chromatogram tandem mass spectrum isotope dilution method
  • Method for simultaneously measuring various drug residues in honey by utilizing liquid chromatogram tandem mass spectrum isotope dilution method
  • Method for simultaneously measuring various drug residues in honey by utilizing liquid chromatogram tandem mass spectrum isotope dilution method

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Embodiment Construction

[0027] The liquid chromatography tandem mass spectrometry isotope dilution method is a method for simultaneously determining multiple drug residues in honey, the method comprising the following steps:

[0028] 1. Extraction

[0029] After the honey sample was diluted with water, it was extracted by adding sodium chloride and acetonitrile. The results showed that the extraction efficiency of acetonitrile for some compounds in quinolones, macrolides and lincosamides was very low, among which orbifloxacin (35) , spiramycin (42), erythromycin (46), lincomycin (51), clincomycin (52) and piricomycin (53) have an extraction efficiency of less than 5%. Acetonitrile cannot effectively extract these compounds from water, so this paper adopts the pretreatment operation of direct solid phase extraction purification for honey samples.

[0030] Specific operation: Weigh 5g sample (accurate to 0.01g) and place it in a 50mL stoppered centrifuge tube, add 0.1mL isotope internal standard solut...

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Abstract

The invention relates to a method for detecting various drug residues in honey, in particular relating to a method for simultaneously measuring various drug residues in honey by utilizing a liquid chromatogram tandem mass spectrum isotope dilution method. The method provided by the invention comprises the following steps: directly diluting by virtue of a phosphate buffer solution the pH value of which is equal to 8; carrying out HLB (Hydrophile Lipophile Balance) extraction and purification; carrying out measurement by utilizing the liquid chromatogram tandem mass spectrum isotope dilution method (LC-MS / MS); and quantifying by utilizing the internal standard method and external standard method of isotope internal standard dilution; and measuring low-limit sulfanilamide drugs to be 1.0 mu g / kg, nitromidazoles drugs to be 1.0 mu g / kg, carbostyril drugs to be 2.0 mu g / kg, macrolide drugs to be 3.0 mu g / kg, lincosamides drugs to be 2.0 mu g / kg and praziquantel to be 0.3 mu g / kg. The method provided by the invention is simple, convenient and rapid and has the advantages of small resource consumption and low detection cost; the front processing procedure, drug variety and instruments for measurement can be better complementary with the existing method; and the method provided by the invention is suitable for the simultaneous measurement requirements of various drugs in the honey andcan provide a powerful technical guarantee for maintaining the food safety and guaranteeing that Chinese honey is successfully exported.

Description

technical field [0001] The invention relates to a detection method for multiple types of drug residues in honey, in particular to a method for simultaneously determining multiple types of drug residues in honey by a liquid chromatography tandem mass spectrometry isotope dilution method. Background technique [0002] In the 1990s, with the integration of the global economy and the internationalization of food trade, food safety has become a worldwide focus, a worldwide challenge and an important global public health problem. Among them, the problem of drug residues affects the safety of animal food It directly affects human health and import and export trade. Monitoring drug residues has become a top priority. Countries around the world have formulated corresponding laws and regulations to limit drug abuse. [0003] Honey is one of the important export products of our country, and it has always been a key product for the detection of various drug residues in various countries...

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 侯建波谢文陈笑梅奚君阳钱艳王峰
Owner THE INSPECTION & QUARANTINE TECH CENT ZHEJIANG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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