加速溶剂萃取-气相色谱-串联质谱法同时测定贝类中64种农药残留

Simultaneous determination of 64 pesticide residues in shellfish by accelerated solvent extraction coupled with gas chromatography-tandem mass spectrometry

建立了加速溶剂同步萃取净化-气相色谱-串联质谱(GC-MS/MS)同时测定贝类中64种农药残留的方法。加速溶剂萃取的萃取溶剂为90%(v/v)乙腈水溶液,萃取温度为85℃、冲洗体积60%萃取池体积、循环次数1次,同时使用0.8 g N-丙基乙二胺(PSA)和0.8 g石墨化炭黑(GCB)在线净化,提取液浓缩定容后,在多反应监测(MRM)模式下测定,外标法定量。结果表明,64种农药在10.0~1000μg/L范围内呈现良好的线性关系,决定系数(r2)均大于0.989,方法的定量限为2.0~10.0μg/kg;对文蛤空白基质进行加标回收试验,添加水平为5.0、10.0和100μg/kg以及定量限水平,得到的平均回收率为69.4%~129.7%,精密度为0.7%~16.0%(n=6)。该方法提取和净化同步完成,操作简单,重复性好,灵敏度高,能够满足于贝类水产品中多种农药残留的同时筛查。

A method was established for the determination of 64 pesticide residues in shellfish using accelerated solvent simultaneous extraction and purification coupled with gas chromatography-tandem mass spectrometry(GC-MS/MS).The target compounds were extracted from shellfish using 90%(v/v)acetonitrile aqueous solution with 60%of the pool volume at 85℃via a single cycle of accelerated solvent extraction.The extracts were synchronously purified with primary secondary amine(PSA)and graphitized carbon black(GCB)added to the extracting cell.After concentration,the target compounds were detected by GC-MS/MS in the multiple reaction monitoring(MRM)mode,and quantified by using the external standard method.Under the optimized conditions,good linearities were obtained for the 64 pesticides in the range of 10.0-1000μg/L,with coefficients of determination greater than 0.989.The limits of quantification for the method were between 2.0μg/kg and 10.0μg/kg.At four spiked levels(5.0,10.0,100μg/kg,and the LOQ level)in clam,the recoveries of all the pesticides were between 69.4%and 129.7%,with the relative standard deviations varying from 0.7%to 16.0%(n=6).The method is simple,repeatable and sensitive,and it is suitable for the screening of various pesticide residues in shellfish products.