气相色谱法测定鱼组织中8种含氟杀虫剂及1种代谢产物残留

Simultaneous analysis of eight fluorine-containing pesticides and one metabolite in fish by gas chromatography

建立了鳗鱼、泥鳅、黄鳝和鲶鱼组织中8种含氟杀虫剂及1种代谢产物气相色谱同时分析的方法。样品组织经过前处理,利用GC-μECD对5种拟除虫菊酯类、氟虫腈及其亚砜、溴虫腈和茚虫威直接进行分析。对前处理过程中的一些细节问题进行了探索。经验证,方法的线性良好,检测限为0.8～3.0μg/kg,定量限为2.5～10.0μg/kg。在3个添加水平下,9种目标化合物在4种组织中的相对标准偏差均小于6.8%,平均回收率在82.0%～98.5%之间。方法已应用于实际样品中目标化合物的筛查,检测出了阳性样本。

This paper developed an efficient method for detection of 8 fluorine-containing pesticides and one metabolite（ bifenthrin,λ-cyhalothrin,cyfluthrin,flucythrinate,tefluthrin,fipronil,fipronil sulfone,chlorfenapyr and indoxacarb） in fish（ eel,catfish,weather loach and monopterus） tissues.After the pretreatment of sample,target compounds were detected by gas chromatography with microelectron capture detection（ GC-μECD） directly.Optimal conditions for the sample pretreatment were investigated.The calibration curves showed good linearity.The limit of detection（ LOD） was 0.8- 3.0 μg/kg,and the limit of quantification（ LOQ） was 2.5 ～10.0 μg/kg.At three spiked levels,the average recoveries for nine compounds in four kinds of tissues ranged from 82.0% to 98.5% with relative standard deviation（ RSD） ≤ 6.8%.This validated method was successfully applied to the determination of the nine compounds in real samples from markets.