气相色谱-三重四级杆质谱法同时测定卷心菜粉中溴虫腈、氟虫腈、联苯菊酯  

Simultaneous determination of chlorfenapyr,fipronil,and bifenthrin in cabbage powder by gas chromatography-triple quadrupole mass spectrometry

作　　者：周梅玲 姚铭栋 李敏洁[1] ZHOU Mei-ling;YAO Ming-dong;LI Minjie(Physical and Chemical Laboratory,Anyang Center for Disease Control and Prevention,Anyang,Henan 455000,China)

机构地区：[1]安阳市疾病预防控制中心理化检验科,河南安阳455000

出　　处：《环境与职业医学》2020年第12期1206-1210,共5页Journal of Environmental and Occupational Medicine

摘　　要：[背景]溴虫腈、氟虫腈、联苯菊酯易残留,对人和动物健康具有潜在危害,目前同时检测三者的方法较少,因此有必要建立一种灵敏、准确的检测方法。[目的]通过优化气相色谱和质谱条件,建立气相色谱-质谱/质谱法同时测定卷心菜粉中溴虫腈、氟虫腈、联苯菊酯。[方法]通过对样品前处理方法中提取溶剂、净化方式的优化,采用气相色谱-三重四级杆质谱,多反应监测模式检测,对质谱测定的目标离子对进行选择,外标法定量。[结果]在以乙腈为提取溶剂,硫酸镁和氯化钠为提取盐,PSA玻璃柱固相萃取的最佳优化条件下,溴虫腈、氟虫腈、联苯菊酯在0.01~0.20 mg·L^(-1)线性范围内,均有良好的线性关系(r>0.998),样品加标回收率分别为84.4%~109.0%、93.4%~106.8%、101.8%~108.2%。相对标准偏差分别为7.3%~8.9%、5.2%~6.9%、4.5%~7.5%。[结论]本法能够实现卷心菜粉中溴虫腈、氟虫腈、联苯菊酯的同时准确测定。[Background]Chlorfenapyr,fipronil,and bifenthrin residues tend to remain in food and have potential hazards to human and animal health.At present,there are few methods to detect the three pesticides at the same time.Therefore,it is necessary to establish a sensitive and accurate detection method.[Objective]This methodological study aims to establish gas chromatography-triple quadrupole mass spectrometry to determine chlorfenapyr,fipronil,and bifenthrin in cabbage powder by optimizing gas chromatography and mass spectrometry conditions.[Methods]After optimizing solvent extraction and purification during pretreatment,gas chromatography-triple quadrupole mass spectrometry in multiple reaction monitoring mode was used to select target ion pairs for determination.The external standard method was also used for quantitative determination.[Results]Under the proposed optimal conditions using acetonitrile as the extraction solvent,magnesium sulfate and sodium chloride as the extraction salts,and PSA glass column solid phase extraction,there were good linear relationships of chlorfenapyr,fipronil,and bifenthrin in the range of 0.01-0.2 mg·L^(-1)(r>0.998);the sample recovery rates were 84.4%-109.0%,93.4%-106.8%,and 101.8%-108.2%,respectively;the relative standard deviations were 7.3%-8.9%,5.2%-6.9%,and 4.5%-7.5%,respectively.[Conclusion]The gas chromatography-triple quadrupole mass spectrometry method can achieve the simultaneous and accurate determination of chlorfenapyr,fipronil,and bifenthrin in cabbage powder.

关 键 词：气相色谱-三重四级杆质谱法 卷心菜粉 农药残留 检测方法 

分 类 号：TS255.7[轻工技术与工程—农产品加工及贮藏工程] O657.63[轻工技术与工程—食品科学与工程]