气相色谱-串联质谱法测定烟草中97种农药残留量
Determination of Residues of 97 Pesticides in Tobacco by GC-MS/MS
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摘要: 利用气相色谱-串联质谱法(GC-MS/MS)检测烟草中97种农药残留。样品以乙腈为溶剂经加速溶剂萃取(ASE),提取液用Carbon-NH2固相萃取小柱净化后,采用VF-5MS色谱柱分离,用电子轰击离子源-多反应监测模式(EI-MRM)检测。97种农药的质量浓度在20~1 000 μg·L-1范围内与其峰面积呈线性关系,方法的测定下限(10S/N)在0.02~22.4 μg·kg-1之间;在50,100,500 μg·kg-1的加标水平下,测得回收率在67.4%~116%之间,测定值的相对标准偏差(n=6)在1.9%~14%之间。Abstract: GC-MS/MS was used to determine residual of 97 pesticides in tobacco. The sample was extracted with acetonitrile by accelerated solvent extraction (ASE). The extract was purified using Carbon-NH2 solid-phase extraction column, separated by GC using VF-5MS column as stationary phase, and detected by MS adopting EI-MRM. Linear relationship between the peak area and the mass concentration of pesticides in the range of 20-1 000 μg·L-1, with limits of quantification (10S/N) in the range of 0.02-22.4 μg·kg-1. Tests for recovery were made by adding of 50, 100, 500 μg·kg-1 of standard samples, giving values of recovery in the range of 67.4%-116% with RSD′s (n=6) in the range of 1.9%-14%.