中草药中有机磷及氨基甲酸酯类农药残留量的GC-MS测定  

Determination of organophosphorous and carbamates pesticide residues in Chinese herbal medicine

作　　者：万益群[1] 李申杰[2] 付贵琴[2] 

机构地区：[1]南昌大学食品科学教育部重点实验室,南昌330047 [2]南昌大学分析测试中心,南昌330047

出　　处：《分析试验室》2007年第6期81-84,共4页Chinese Journal of Analysis Laboratory

基　　金：长江学者和创新团队发展计划(IRT0540);江西省自然科学基金(0420039);南昌大学食品科学教育部重点实验室开放基金(NCU200408)项目资助

摘　　要：气相色谱-质谱法同时测定中草药中多种有机磷及氨基甲酸酯类农药残留量.采用V（乙腈）∶V（丙酮）＝3∶7混合溶剂微波辅助提取,弗罗里硅土和中性氧化铝层析柱净化,气相色谱-质谱（GC-MS）联用检测,农药混标在0.01～1.0 μg/mL范围内线性良好,在0.5、0.1、0.05 μg/mL 3个水平添加平均回收率分别为86.5%～110.6%、81.2%～108.3%和72.9%～122.3%,相对标准偏差分别为2.6%～8.3%、4.6%～9.7%和2.3%～10.7%.To make a simultaneous determination of organophosphorous and carbamates pesticide residues in Chinese herbal medicine by gas chromatography-mass spectrometry. The pesticide residues were extracted from Chinese herbal medicine with solvents by microwave assisted extraction; Extracts were cleaned up with a column filled with Flofisil and neutral aluminum oxide, and analyzed with gas chromatography-mass spectrometry. The results presented the excellent linearity between analytical signal and analyte concentration in the range of 0.01 - 1.0 μg/mL; The recoveries obtained from samples spiked with standards at the concentration levels of 0.5, 0.1 and 0.05 μg/mL were in the ranges of 86.5% - 110.6%, 81.2% - 108.3% and 72.9% - 122.3%, respectively, with relative standard deviations of 2.6% - 8.3%, 4.6% -9.7% and 2.3% - 10.7%, respectively. The method can be used for simultaneous determination of pesticide residues in Chinese herbal medicine.

关 键 词：气相色谱-质谱法 微波辅助萃取 中草药 有机磷农药 氨基甲酸酯类农药 

分 类 号：O657.63[理学—分析化学]