通过对QuEChERS(Quick,Easy,Cheap,Effective,Rugged and Safe)方法的改良,建立了9种中草药中13种代表性农药残留分析的气相色谱-串联质谱分析方法。新鲜样品用乙腈提取,干样品用水和乙腈提取,再加入NaCl和无水MgSO4液液分离;然后,在新鲜样品提取液中加入无水MgSO4和多壁碳纳米管,在干样品提取液中加入无水MgSO4、多壁碳纳米管和N-丙基二乙胺(Primary secondary amine,PSA),进行分散固相净化。采用气相色谱分离、选择离子监测质谱进行确证和测定,内标法定量。3个添加水平(0.02~0.4 mg/kg)的平均回收率为67.9%~100.3%,相对标准偏差为0.6%~11.0%;方法定量限(LOQ)在0.004~0.03 mg/kg之间;检出限(LOD)在0.009~0.01 mg/kg之间。采用本方法检测12例市场样品,其中3例样品检测出目标农药。
A simple method for the determination of 13 representative pesticides in 9 Chinese herds employing modified QuEChERS(Quick,Easy,Cheap,Effective,Rugged and Safe) followed by gas chromatography-tandem mass spectrometric(GC-MS) analysis was developed.For the fresh or dry samples,the pesticides were extracted by acetonitrile or acetonitrile-H2O,respectively,and then liquid-liquid partitioning formed by adding anhydrous MgSO4 and NaCl;followed by a simple cleanup step using multi-walled carbon nanotubes(MWCNTs) for fresh samples extraction,and using MWCNTs and PSA(primary secondary amine) for dry samples extraction as dispersive solid phase extraction(d-SPE).The aliquot was confirmed and determined by gas chromatography with selected ion monitoring mode(SIM)-mass spectrometry.The recoveries for all the pesticides studied were from 67.9% to 100.3% with relative standard deviation(RSD) from 0.6% to 11.0% in the concentration range of 0.02-0.4 mg/kg.The limit of quantitation(LOQ) was from 0.004 mg/kg to 0.03 mg/kg,and the limit of detection(LOD) was from 0.009 mg/kg to 0.01 mg/kg.Three positive market samples,polluted by target pesticides,were screened by the developed method.