摘要
目的建立气相色谱-三重四级杆质谱法(gas chromatography-triple quadrupole mass spectrometry,GC-MS/MS)对农药制剂中32种隐性添加农药成分的分析方法。方法样品采用丙酮直接提取,正己烷定容,内标法定量,气相色谱-串联质谱仪检测。结果 32种农药的平均添加回收率为71.51%~100.88%,相对标准偏差(relative standard deviation,RSD)为1.36%~7.43%,检出限为0.03%~0.17%,定量限为0.1%~0.5%。采用建立的方法对抽检的农药产品进行检测,结果表明部分农药中检出隐性成分,在0.5%的苦参碱水剂中检出1.6%的氰戊菊酯,在5%的高效氯氟氰菊酯中检出3.5%的氟虫腈。结论该方法高效、准确,可用于同时测定农药中的32种隐性添加农药成分。
Objective To establish a method for determination of 32 kinds of implicitly added ingredients in pesticide formulations by gas chromatography-triple quadrupole mass spectrometry（GC-MS/MS）.Methods The samples were directly extracted with acetone,and volumed with n-hexane.Then they were detected by GC-MS/MS and quantified by internal standard method.Results The average recoveries of 32 kinds of pesticides were 71.51%-100.88% and the relative standard deviations（RSDs） were 1.36%-7.43%.The limits of detection were 0.03%-0.17%,and the limits of quantification were 0.1%-0.5%.The established method was used to detect pesticide products,and the results showed that some of the pesticides were detected in recessive ingredients.Totally 1.6% of fenvalerate was detected in 0.5% of matrine aqueous solution,and 3.5% of fipronil was detected in 5% of lambda-cyhalothrin.Conclusion The method is efficient and accurate,which can be used for simultaneous determination of 32 kinds of implicitly added ingredients in pesticides.
作者
李俊
蔡滔
周雪丽
卢平
吴玉娥
刘佳
陈会
王震
庞宏宇
王艺蓉
罗华兰
LI Jun;CAI Tao;ZHOU Xue-Li;LU Ping;WU Yu-E;LIU Jia;CHEN Hui;WANG Zhen;PANG Hong-Yu;WANG Yi-Rong;LUO Hua-Lan(Guizhou Provincial Supervision and Testing Center for Agricultural Product Quality, Guiyang 550004, China;Agricultural Products Quality and Safety Risk Assessment Laboratory of Ministry of Agriculture （ Guiyang）, Guiyang 550004, China;Key Laboratory of Green Pesticide and Agricultural Bioengineering, Ministry of Education, Center for Research and Development for Fine Chemicals, Guizhou University, Guiyang 550025, China)
出处
《食品安全质量检测学报》
CAS
2018年第13期3219-3225,共7页
Journal of Food Safety and Quality
基金
国家自然科学基金项目(21507016)
国家农产品风险评估项目(GJFP2017005)
2017年贵州省地方标准制修订项目~~
关键词
隐性添加
农药
气相色谱-三重四级杆质谱法
implicitly added
pesticide
gas chromatography-triple quadrupole mass spectrometry
