高效液相色谱-串联质谱法测定稻渔土壤中氟虫腈及其代谢物残留  

Determination of Fipronil and Its Metabolites in Paddy-fish Soil Using High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：马丽莎[1] 谢文平[1] 尹怡[1] 单奇[1] 刘书贵[1] 李丽春[1] 赵成 戴晓欣[1] 魏林婷 郑光明[1] MA Li-sha;XIE Wen-ping;YIN Yi;SHAN Qi;LIU Shu-gui;LI Li-chun;ZHAO Cheng;DAI Xiao-xin;WEI Lin-ting;ZHENG Guang-ming(Key Laboratory of Recreational Fisheries Research,Ministry of Agriculture,Minisitry of Agriculture Laboratory of Quality&Safety Risk Assessment for Aquatic Product(Guangzhou),Pear River Fisheries Research Institute,Chinese Academy of Fishery Sciences,Guangzhou 510380,China)

机构地区：[1]中国水产科学研究院珠江水产研究所,农业部水产品质量安全风险评估实验室(广州),农业部休闲渔业重点实验室,广东广州510380

出　　处：《质谱学报》2021年第6期1025-1032,共8页Journal of Chinese Mass Spectrometry Society

基　　金：国家水产品质量安全风险评估-稻渔综合种养水产品安全性评估(GJFP201800902);广东省渔业生态环境重点实验室开放基金(FEEL-2020-8);中国-东盟海上合作基金(CAMC-2018F)。

摘　　要：建立了高效液相色谱-串联质谱(HPLC-MS/MS)法测定稻渔土壤中氟虫腈及其代谢物残留。样品经乙腈恒温振荡提取,ENVI-18固相萃取柱和10 mg GCB净化,ZORBAX Extend-C18色谱柱(2.1 mm×100 mm×1.8μm)分离,电喷雾负离子模式检测,基质匹配标准曲线外标法定量。结果表明,稻渔土壤中氟虫腈、氟甲腈、氟虫腈砜和氟虫腈亚砜的平均回收率在83.5%~110.3%之间,相对标准偏差在1.9%~11.5%之间,氟虫腈及其代谢物在0.5~100μg/L浓度范围内的线性关系良好,相关系数均大于0.998,检出限和定量限分别为1.0、3.0μg/kg。该方法操作简单、结果准确、可靠,可实现样品的批量化处理,能够满足稻田水产品中氟虫腈及其代谢物检测的需求。Residues of fipronil and its metabolites in paddy-fish soil were detected using high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Samples were extracted with oscillation and acetonitrile in constant temperature,and subsequently purified by solid phase extraction using ENVI-18 column and 10 mg GCB.The target compounds were separated on an Agilent ZORBAX Extend-C18 column(2.1 mm×100 mm×1.8μm),and determined using electrospray ionization(ESI)source at negative mode with multiple reation monitoring(MRM).The analytes were quantified with external standard using the matrix-matched standard calibration curve method.The results indicated that the average spiked recoveries of fipronil,fipronil-desulfinyl,fipronil-sulfone and fipronil-sulfide in paddy-fish soil were 83.5%-110.3%with the relative standard deviations(RSDs)of 1.9%-11.5%.Good linearities were obtained in the range of 0.5-100μg/L,and the correlation coefficients were greater than 0.998,the limits of detection(LODs)were 1.0μg/kg,and the limits of quantification(LOQs)were 3.0μg/kg.This method is simple,accurate and reliable,which can meet the detection requirements of fipronil and its metabolites in paddy-fish soil.

关 键 词：高效液相色谱-串联质谱(HPLC-MS/MS) 恒温振荡 稻渔土壤 氟虫腈 氟甲腈 氟虫腈砜 氟虫腈亚砜 

分 类 号：O657.63[理学—分析化学]