固相萃取-气相色谱-质谱法测定饮用水中36种农药残留量

GC-MS Determination of Residual Amounts of 36 Pesticides in Drinking Water with Enrichment by Solid Phase Extraction

提出了固相萃取-气相色谱-质谱联用法测定饮用水中36种农药的残留量。样品用石墨化碳/氨基复合型小柱净化和富集后,经DB-1701P弹性石英毛细管柱分离,用电子轰击离子源及选择离子监测扫描模式进行质谱测定。36种农药在一定浓度范围内呈线性关系,检出限(3S/N)在0.001 3～0.070mg.L-1之间。按方法在水样的基础上加入农药混合标准溶液做回收试验,测得回收率在90.8%～112.4%之间,测定值的相对标准偏差(n=5)在3.20%～13.2%之间。

GC-MS with enrichment by solid phase extraction was applied to the determination of residual amounts of 36 pesticides in drinking water.The sample was purified and enriched by passing through graphitized carbon/amino-compound column.DB-1701P elastic quartz capillary column was used for separation,and EI source with SIM mode was used in MS determination.Linearities for the 36 pesticides were obtained in definite concentration ranges,with values of detection limits（3S/N） ranged from 0.001 3-0.070 mg·L-1.Following the proposed method test for recovery was made by addition of mixed standard of the pesticides,values of recovery obtained were in the range of 90.8%-112.4%,with RSD′s（n=5） in the range of 3.20%-13.2%.