白芍和黄连中十五种有机氯和拟除虫菊酯类 农药的多残留分析方法

建立了白芍和黄连两种中药材中六六六、滴滴涕、艾氏剂、五氯硝基苯、甲氰菊酯、氯菊酯、氯氰菊酯、氰戊菊酯、溴氰菊酯等农药的多残留气相色谱分析方法。在索氏提取器中以石油醚(60~90℃)为溶剂提取样品,提取液经氧化铝与弗罗里硅土的混合柱净化,采用农残分析专用柱农残Ⅱ 柱分离,GC-ECD检测器检测农药的残留量。方法的最小检出量(LOD)为0.000 5~0.006 0 ng, 最低检测浓度(LOQ)为0.005~0.050 mg/kg;3个添加水平农药的平均回收率为79.8％~114.6％,相对标准偏差(RSD)均小于10％ (n=6) 。

Multi-residue Analysis of Fifteen Organochlorine and Pyrethroid Insecticides in Raidix paeoniae Alba and Rhizoma coptidis

A method for rapid determination of fifteen organochlorine and pyrethroid insecticide residues (included α-HCH,β-HCH,γ-HCH,δ-HCH,p,p'-DDE,o,p'-DDT,p,p'-DDD,p,p'-DDT,PCNB,aldrin, fenpropathrin, permethrin,cypermethrin,fenvalerate,deltamethrin) in two kinds of Chinese crude drugs (Raidix paeoniae Alba and Rhizoma coptidis) were developed.The sample was extracted in Soxhlet with petroleum ether (60~90°C) and cleaned up with the mixture of aluminum oxide-florisil (5 g and 7 g),detected by GC-ECD.The limit of detection (LOD) of 15 organochlorine and pyrethroid insecticides were 0.000 5~0.006 0 ng,and the limit of quantitation (LOQ) of the method for 15 organochlorine and pyrethroid insecticides in Raidix paeoniae Alba and Rhizoma coptidis were 0.005~0.050 mg/kg,and fortified recovery of pesticides at three levels were 79.8%~114.6%, the RSD were below 10% (n=6).