气相色谱-质谱法测定水产品中氟胺氰菊酯残留量

本文建立了水产品中氟胺氰菊酯残留量的气相色谱-质谱测定方法。样品经正己烷-丙酮（体积比2：1）超声提取、冷冻除脂、中性氧化铝固相萃取柱净化后，用气相色谱-质谱法进行测定和确认，外标法定量。在优化实验条件下，氟胺氰菊酯在10．0～400．0μg·L^-1范围内线性关系良好，相关系数为0．9999，检出限为2．0μg·kg^-1，定量限为4．0μg·kg^-1。在4．0、8．0和40．0μg·kg^-1加标水平下，鲤（Cyprinus carpio）、草鱼（Ctenopharyngodon ideUus）和凡纳滨对虾（Penaeus vannamei Boone）可食部分为基质的平均回收率为87．92％～98．37％，相对标准偏差为0．96％～4．97％。该方法操作简单、灵敏度高、净化效果理想、重珊陛好，可满足水产品中氟胺氰菊酯的定性定量检测的要求。

Detection of Tau-Fluvalinate Residues in Fishery Products by Gas Chromatography-Mass Spectrometry

A gas chromatography-mass spectrometry （GC-MS） method was developed for the determination of tau-fluvalinate in fish- cry products, In the method, the sample was ultrasound-assisted extracted by n-hexane-acetone- （2 ： 1 ）, freeze-degreased, and cleaned up with neutral aluminum oxide solid phase extraction column. The determination was performed by GC-MS while quantificatlon was performed by the external standard method. Under the optimal conditions, the calibration curve showed a good linearity in the range of 10.0~400.0 μg·kg^-1 for tau-fluvalinate with a correlation coefficient of 0.9999. The limit of detection for tau-fluvalinate was 2.0 μg·kg^-1 and the limit of quantitaion was 4.0μg·kg^-1. The recovery rates of tau-fluvalinate was ranged from 87.92% to 98.37% with relative standard deviations （RSDs, n=6） of 0.96% to 4.97% in common carp （Cyprinus carpio）, grass carp （Ctenopharyngodon idellus ）and Pacific white leg shrimp （Penaeus vannamei Boone） at three spiked concentration levels of 4.0, 8.0 and 40.0 μg·kg^-1. It is concluded that the method could meet the requirements for the determination of tau-fluvalinare residues in fishery products due to the advantages of simple, sensitive and high cleanup effectiveness, and good reproducibility.