QuEChERS-液相色谱-串联质谱法测定鲤肝脏中氟虫腈及其代谢物残留

以QuEChERS作为样品前处理方法,结合高效液相色谱-串联质谱(HPLC-MS/MS)检测技术,建立了鲤(Cyprinus carpio)肝脏中氟虫腈(fipronil)及代谢物氟甲腈(fipronil desulfinyl)、氟虫腈亚砜(fipronil sulfide)和氟虫腈砜(fipronil sulfone)的检测方法。样品用0.1%甲酸乙腈提取,提取液经吸附剂中性氧化铝、乙二胺-N-丙基硅烷(PSA)结合石墨炭化黑粉(GCB)净化,以LC-MS/MS进行测定,基质匹配标准曲线外标法定量。结果表明,鲤肝脏中4种目标物的平均回收率在87.3%~109.2%之间,相对标准偏差在1.3%~12.0%之间,氟虫腈及其代谢物在0.4~100.0 ng/mL线性范围内,线性良好,线性相关系数(r2)均大于0.997,检出限为2.0μg/kg,定量限为5.0μg/kg。该方法简单、快速且灵敏,单个样品前处理仅需20 min,适用于鲤肝脏中氟虫腈药物代谢及残留消除规律研究。

Determination of Fipronil and Its Metabolites in Liver Tissue of Cyprinus carpio by QuEChERS Combined with Liquid Chromatography-Tandem Mass Spectrometry

A determination method of fipronil and its metabolites(fipronil desulfinyl,fipronil sulfide and fipronil sulfone)in liver tissue of Cyprinus carpio was developed by quick,easy,cheap,effective,rugged,and safe(QuEChERS)extraction coupled with high performance liquid chromatography-tandem mass spectrometry(LC-MS/MS).Samples were extracted with 0.1%formic acid acetonitrile,and purified by neutral alumina,PSA and GCB.Then,fipronil and its metabolites were detected by using LC-MS/MS.The analytes were quantified with external standard using the matrix-matched standard calibration curve method.The results showed that the average spiked recoveries of fiproni and its metabolites in liver tissue of fish were 87.3%~109.2%with relative standard deviations(RSDs)of 1.3%~12.0%.Good linearities were obtained in the range of 0.4~100.0 ng/mL,and the correlation coefficients were greater than 0.997,the LODs were 2.0μg/kg,and the LOQs were 5.0μg/kg.The method was simple,rapid and sensitive.And the preparation for a single sample was within 20min.The developed method is suitable for studying the metabolism and residue elimination of fipronil in fish liver.