气相色谱-质谱法测定高粱籽粒中11种有机磷农药残留量
GC-MS Determination of Residual Amounts of 11 Organophosphorus Pesticides in Sorghum Seeds
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摘要: 提出了气相色谱-质谱法同时测定高粱籽粒中11种有机磷农药含量的方法。高粱样品加水浸湿后,用乙腈提取,依次用C18固相萃取柱和Carb/PSA柱净化。采用HP-5MS色谱柱分离,选择离子监测模式测定,外标法定量。11种有机含磷农药的质量浓度均在0.05~1.0 mg·L-1范围内呈线性,检出限(3S/N)在0.001~0.025 mg·kg-1之间。加入2个浓度水平标准溶液进行回收试验,所得回收率在81.3%~108%之间,测定值的相对标准偏差(n=5)在1.5%~8.0%之间。Abstract: GC-MS was applied to the determination of residual amounts of 11 organophosphorus pesticides in sorghum seeds. The sample was sopped with H2O and extracted with acetonitrile, the extract was purified by C18 SPE column and Carb/PSA column. The eluate was taken for separation on HP-5MS chromatographic column and the contents of 11 organophosphorus pesticides were determined under SIM mode. External standard method was adopted in the determination. Linear relationships between values of peak area and mass concentration of the 11 organophosphorus pesticides were obtained in the range of 0.05-1.0 mg·L-1, with their detection limits (3S/N) in the range of 0.001-0.025 mg·kg-1. Test for recovery were made by addition of standard at 2 different concentration levels, values of recovery found were in the range of 81.3%-108%, with values of RSD′s (n=5) in the range from 1.5% to 8.0%.