固相萃取-气相色谱双塔双柱法同时测定中药材中53种有机磷类农药残留量

Solid phase extraction-gas chromatography with dual tower and dual column for the simultaneous determination of 53 organophosphorus pesticides in traditional Chinese herbal medicines

目的:研究中药材中有机磷类农药残留量的测定方法。方法:选用代表性的白果、人参、肉桂、红花、银杏叶、广藿香等中药材样品进行研究,样品经高速均质器均质提取,依次经C18固相萃取柱、石墨化碳/氨基串联固相萃取柱(SPE)净化后,用气相色谱双塔双柱进样,双火焰光度检测器(或氮磷检测器)同时定性、定量测定。结果:在6种中药材样品基质、三水平添加条件下,53种农药的回收率大多在70.0%～120.0%,相对标准偏差小于15%,检测限大多低于0.01mg/kg,符合农药多残留检测的要求。结论:本法净化效果好,基质干扰小,灵敏度高,重现性好,可用于中药材样品中有机磷类农药残留量的日常检测。

AIM： The multi-residues method was used to determine organophosphorus pesticides in traditional Chinese herbal medicines （TCHMs）. METHODS： Fifty three pesticides were extracted by high-speed homogenization, and then cleaned sequentially by C18 and Carb/NH2 solid phase extraction （SPE） cartridges. The residues were simultaneously identified and quantified by GC-FPD equipped with dual tower, dual column and two FPD detectors. RESULTS： The analytical performance was demonstrated by the analysis of 6 TCHMs samples extracts, spiked at three concentration levels for each pesticide. In general, the recoveries ranging from 70% to 120% , with relative standard deviations （RSDs） less than 15%, were obtained. The limit of detection （LOD） for most of the targeted pesticides tested was below 0.01 mg/kg. CONCLUSION： The method has good extraction efficiency, purification effect and good reproducibility, which can be applied to the determination of organophosphorus pesticide residues in the routine analysis of TCHMs.