气相色谱-质谱联用法同时测定中药材中53种农药残留方法

 目的 采用气相色谱-质谱法研究中药材中农药多残留的测定方法。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，样品经乙腈匀浆萃取，依次经碳十八、石墨化碳与氨丙基串联固相萃取小柱净化后，采用气相色谱-质谱同时定性、定量测定。结果 在6种中药材样品基质、3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20％，检测限大多低于0.01 mg·kg^-1，符合农药多残留检测的要求。结论 本法净化效果好，灵敏度高，重现性好，可用于中药材样品中农药多残留的日常检测。

Simultaneous Determination of 53 Pesticide Residues in Traditional Chinese Herbal Medicines by GC/MS

OBJECTIVE To develop the multi-residues methods for traditional Chinese herbal medicines(TCHMs) by GC-MS. METHODS 6 representative samples（Semen Ginkgo，Radix Ginseng，Cortex Cinnamomi，Flos Carthami， Folium Ginkgo，and Herba Pogostemonis）were selected as experimental materials. The selected samples were extracted by acetonitrile， and then cleaned by C₁₈ and Envi-carb/PSA solid phase extraction (SPE) cartridges. The residue detection was carried out by GC-MS. RESULTS The analytical performance was demonstrated by the analysis of 6 TCHMs samples' extracts， fortified at three levels for each pesticide. In general， the recoveries ranged from 70% to 120% and relative standard deviations (RSDs) were all less than 20%. The limits of detection (LODs) for most of the selected pesticides were below 0.01 mg·kg^-1. CONCLUSION The method shows high sensitivity，good repeatability and satisfactory cleaning-up excellence， which could be applied to the pesticide residue detection for the TCHMs.