超高效液相色谱-串联质谱法测定畜禽毛发中氟虫腈及其代谢物残留量

Determination of fipronil and its metabolites in animal hair by ultra-high performance liquid chromatography-tandem mass spectrometry

建立了一种测定畜禽毛发中氟虫腈及其代谢物残留量的检测方法。1%十二烷基硫酸钠或5%吐温80清洗毛发,3 m L乙腈溶液和3 m L水混合提取,经涡旋、水浴震荡和超声,采用乙二胺-N-丙基硅烷(PSA)和十八烷基硅烷(C18)基质分散净化,Agilent ZORBAX Eclipse Plus C18色谱柱分离,负离子扫描,电喷雾串联质谱多反应监测模式测定。氟虫腈及其代谢物在毛发中线性关系良好(R^2>0.99),在0.5,1.0,5.0μg/kg 3个添加水平下毛发中氟虫腈、氟甲腈、氟虫腈砜、氟虫腈亚砜的回收率分别为89.1%~107.4%、77.0%~78.9%、73.6%~85.8%和70.9%~80.0%,相对标准偏差均小于6.8%,检出限和定量限分别为0.2和0.5μg/kg。该方法适合于畜禽毛发中氟虫腈及其代谢物残留量的测定。

A method of ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was developed to detected fipronil and its metabolites in animal hair.In the method,hair was washed with1%sodium dodecyl benzene sulfonate or 5%Tween 80,extracted with 3 m L acetonitrile solution and 3 m L water,vortexed,vibrated and ultrasound,then purified with ethylamine n-propyl silane(PSA)and octadecyl silane(C18).The reconstituted sample solution was analyzed by UPLC-MS/MS in negative mode,with Agilent ZORBAX Eclipse Plus C18 column as the separation column.Fluoronitrile and its metabolites had a good linear relationship in the hair samples(R^2>0.99),and the recoveries of fipronil,desulfinyl,sulfone and sulfide at0.5,1.0 and 5.0μg/kg levels were 89.1%to 107.4%,77.0%to 78.9%,73.6%to 85.8%and 70.9%to80.0%,respectively.The relative standard deviation was less than 6.76%,and the detection limit and quantification limit were 0.2 and 0.5μg/kg,respectively.The method is suitable for the determination of fipronil and its metabolites in animal hair.