QuEChERS-高效液相色谱-串联四极杆飞行时间质谱法同时测定大米中7种除草剂残留

Simultaneous determination of seven herbicide residues in rice using QuEChERS-high performance liquid chromatography-tandem mass spectrometry Triple TOF

建立了同时测定大米中西草净、异丙隆、苄嘧磺隆、莎稗磷、乙氧氟草醚、草酮和二甲戊灵7种除草剂残留的QuEChERS-高效液相色谱-串联四极杆飞行时间质谱(HPLC-MS/MS Triple TOF)方法。样品经V (乙酸乙酯):V (水)=80:20混合溶液提取,以N-丙基乙二胺(PSA)为吸附剂进行基质分散萃取净化,采用HPLC-MS/MS Triple TOF检测,外标法定量。结果表明:7种除草剂在一定的质量浓度范围内,其峰面积与对应的质量浓度间线性关系良好,相关系数均大于0.99;西草净、异丙隆、苄嘧磺隆和莎稗磷在0.001、0.01、0.05 mg/kg 3个添加水平下的平均回收率在75%~108%之间,相对标准偏差(RSD)在1.1%~7.0%(n=5)之间,定量限(LOQ)均为0.001 mg/kg;乙氧氟草醚、草酮和二甲戊灵在0.01、0.05和1 mg/kg 3个添加水平下的平均回收率在81%~108%之间,RSD在2.7%~9.0%之间,LOQ均为0.01 mg/kg。该方法样品前处理简单快速,方法灵敏度、准确度和精密度均符合农药残留检测要求,可用于大米中西草净、异丙隆、苄嘧磺隆、莎稗磷、乙氧氟草醚、草酮和二甲戊灵残留的同时检测。

A multi-residue method was established to simultaneously determine seven herbicides(simetryn,isoproturon,bensulfuron methyl,anilofos,oxyfluorfen,oxadiazon and pendimethalin)in rice using QuEChERS and high performance liquid chromatography-tandem mass spectrometry Triple TOF(HPLC-MS/MS Triple TOF).The samples were extracted with a mixture of ethyl acetate and water(Vethyl acetate:Vwater=80:20),purified by dispersive solid phase extraction with primary secondary amine(PSA),and detected by HPLC-MS/MS Triple TOF using the external standard method for quantitative analysis.Good linearity was achieved with a correlation coefficient of 0.99.The average recoveries of simetryn,isoproturon,bensulfuron methyl and anilofos ranged from 75%to 108%with the spiked levels of 0.001,0.01 and 0.05 mg/kg.And the relative standard deviation(RSD)ranged from1.1%to 7.0%(n=5).The limits of quantification(LOQs)of all those herbicides were 0.001 mg/kg.The average recoveries of oxyfluorfen,oxadiazon and pendimethalin ranged from 81%to 108%with the spiked levels of 0.01,0.05 and 1 mg/kg.And the RSD ranged from 2.9%to 9.0%(n=5).And their LOQs were 0.01 mg/kg.This method is simple and rapid.Its sensitivity,accuracy and precision can meet the requirements of the pesticide residue analysis.Therefore,this method can be applied to the simultaneous analysis of simetryn,isoproturon,bensulfuron methyl,anilofos,oxyfluorfen,oxadiazon and pendimethalin in rice.