QuEChERS-高效液相色谱-串联质谱法测定鲤鱼和小龙虾中毒氟磷残留

Determination of dufulin residues in carp and crayfish by QuEChERS-high performance liquid chromatography-tandem mass spectrometry

建立了鲤鱼和小龙虾中毒氟磷残留的QuEChERS-高效液相色谱-串联质谱检测方法。样品经乙腈提取,采用50 mg乙二胺-N-丙基硅烷(PSA)、50 mg十八烷基键合硅胶(C18)和50 mg无水硫酸镁分散萃取净化,以Eclipse XDB-C18色谱柱分离待测物,采用电喷雾离子化正离子扫描和多反应监测模式(MRM)检测,以空白基质匹配标准溶液外标法定量。结果表明:在1.0~50μg/L范围内,毒氟磷质量浓度与相应的峰面积间呈良好线性关系,相关系数均大于0.999,其在鲤鱼和小龙虾中的检出限(LOD)分别为0.4和0.8μg/kg,定量限(LOQ)分别为2和3μg/kg;在10、50和100μg/kg添加水平下,鲤鱼和小龙虾2种基质中毒氟磷的日内和日间回收率为88%~103%,相对标准偏差(RSD)为1.2%~5.4%。该方法操作简便、经济、环保,能够满足鲤鱼和小龙虾中毒氟磷快速检测要求。

A rapid method for the determination of dufulin residues in the carp and crayfish by QuEChERS-high performance liquid chromatography-tandem mass spectrometry was developed.The samples were extracted with acetonitrile,and cleaned up by 50 mg PSA,50 mg C18 and 50 mg MgSO4.The samples were separated on a Eclipse XDB-C18 column,and detected under positive polarity multiple reactions monitoring(MRM)mode.The matrix matched external standard calibration curves were used for quantitative analysis.The result indicated that the good linearities of dufulin was in the concentration range of 1.0-50μg/L with correlation coefficients higher than 0.999.At the fortified levels of 10,50 and 100μg/kg,the average recoveries of dufulin in the carp and crayfish,were in the range of88%-103%,with intra-and inter-day relative standard deviations varies from 1.2%to 5.4%.The limit of detections(LOD)for carp and crayfish were 0.4 and 0.8μg/kg,respectively.And the limit of quantifications(LOQ)of dufulin for them were 2 and 3μg/kg,respectively.This method was simple,accurate,economic and friendly to the environment,which could meet the requirements for rapid determination of dufulin residues in the carp and crayfish.