气相色谱质谱测定三七、云木香、茯苓中有机磷农药残留量方法研究  

Study on determination of eight organophosphate pesticides residues from Panax Notoginseng,Aucklandia Lappa Decne and Poria Cocos by Gas Chromatography /Mass Spectrometry

作　　者：刘卫[1,2,3] 吴娜[1,2,3] 潘青山[1,2,3] 樊爱萍[1,2,3] 严和平[1,2,3] 陈显兰[1,2,3] 周波[1,2,3] 石玲[1,2,3] 徐世娟[1,2,3] 

机构地区：[1]云南红河学院理学院化学系,云南蒙自661100 [2]云南红河学院理学院分析测试中心,云南蒙自661100 [3]云南省高校天然药物与化学生物学重点实验室,云南蒙自661100

出　　处：《食品工业科技》2013年第17期303-306,共4页Science and Technology of Food Industry

基　　金：国家公益行业项目(200810998);云南省应用基础研究计划青年项目(2012FD053)

摘　　要：采用气相色谱质谱（GC／MS）建立三七、云木香、茯苓中的8种有机磷类农药（甲胺磷、敌敌畏、乙酰甲胺磷、敌百虫、乐果、乙拌磷、甲基对硫磷和毒死蜱）残留量的快速检测方法。样品经过丙酮超声提取，提取液经过C18固相萃取小柱净化，乙酸乙酯和正己烷的混合溶液（体积比为5：5混合）为洗脱液洗脱，洗脱液浓缩尽干后乙腈定容，于GC／MS上检测。对样品前处理条件进行了优化，采用选择离子扫描（SIM）方式，外标法定量。8种有机磷类农药在0.05～5μg／mL范围内线性良好。相关系数为0.9910～0.9994，平均加标回收率为71.03％～115.57％，相对标准偏差（RSD，n=3）为0.54％～9.36％，检出限（S／N=3）在2.8×10^-6～4.0×10^-5μg之间。结果表明，该方法简便、快速，能满足三七、云木香、茯苓中8种有机磷类农药残留量同时测定的要求。A rapid analytical method has been developed for determination of eight Organophosphate Pesticides （Methamidophos, Dichlorovos, Acephate, Frichlorfon, Dimethoate, Disulfoton, Parathion - methyl, Chlorpyrifos） Residues from Panax Notoginseng, Aucklandia Lappa Decne and Poria Cocos by Gas Chromatography/Mass Spectrometry（GC/MS）.The sample was extracted with acetone as the extraction by means of ultrasonication.The crude extract was purified by an C 18solid phase extraction column,which was eluted from homogenized tissue with ethylacetate-n-hexane（5：5,v/v）.The eluates were concentrated,and then were redissolved in acetonitrile prior to GC/MS analysis.Sample pre-treatment conditions were optimized.The determination was performed in selected ion monitoring （SIM）mode with the external calibration for quantitative analysis. The linear range of eight organophosphate pesticides was 0.05-51μg/mL, the correlation coefficients were 0.9910-0.9994, the average recoveries ranged from 71.03% to 115.57%, and the relative standard deviation（ RSD, n = 3） were between 0.54% and 9.36% ,the limits of detection （S/N = 3）were 2.8 × 10^-6-4.0 × l0^-5μg.The results indicated that the method developed was easier and faster. It also demonstrated that this multiresidue analysis method could meet the requirements for simultaneous determination of many organophosphate pesticides in Panax Notoginseng, Aucklandia Lappa Decne and Poria Cocos.

关 键 词：气相色谱质谱 三七 云木香 茯苓 有机磷类农药 

分 类 号：TS207.3[轻工技术与工程—食品科学]