全自动凝胶渗透色谱法净化-气相色谱-串联质谱法测定茄果类蔬菜中7种有机磷类杀虫剂残留量  

Determination of 7Organophosphorus Pesticide Residues in Solanaceous Vegetables by GC-MS/MS after Purification with Automatic GPC

作　　者：宁方尧[1] NING Fangyao(Guangxi Vocational&Technical Institute of Industry,Nanning 530000,China)

机构地区：[1]广西工业职业技术学院,南宁530000

出　　处：《理化检验（化学分册）》2021年第5期476-480,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：将茄果类蔬菜样品用乙腈萃取后,采用全自动凝胶渗透色谱法(GPC)净化-气相色谱-串联质谱法(GC-MS/M S)测定茄果类蔬菜中7种有机磷类杀虫剂(抑菌灵、毒死蜱、氟菌唑、百菌清、噻菌灵、敌菌灵和戊菌唑)残留量。优化的GPC条件为:体积比1∶4的丙酮-环己烷混合溶液为洗脱剂,流量为5mL·min^(-1),洗脱时间为8min,收集时间为6min;优化的测定条件为:HP-5MS型色谱柱为分离柱,选择电子轰击离子(EI)源和多反应监测(MRM)模式,以环氧七氯为内标物。结果显示:7种有机磷类农药工作曲线的线性范围均为0.05~5.0mg·L^(-1),检出限(3S/N)为0.0022~0.0045mg·kg^(-1)。按标准加入法进行回收试验,回收率为94.2%~103%,测定值的相对标准偏差(n=6)均小于5.0%。The sample of solanaceous vegetables was extracted with acetonitrile,and the residual contents of 7 organophosphorus pesticides(i.e.,dichlofluanid,chlorphrifos,t riflumizole,chlorothalonil,thiabendazole,anilazine,and penconazole)in the purified solution were determined by GC-MS/MS after purification by Autonatic GPC.The optimized conditions of GPC were found:the mixture of acetone and cyclohexane with the volume ratio of 1∶4used as eluent,the flow rate of 5mL·min^(-1),the elution time of 8min,and the collection time of 6min.The optimized conditions of determined conditions were found:HP-5MS chromatographic column used as separated column,EI and MRM mode adopted in MS/MS analysis,heptachlor epoxide used as internal standard.As found by results,linearity ranges of the standard curves of 7organophosphorus pesticides were within 0.05-5.0mg·L^(-1),with detection limits(3 S/N)in the range of 0.0022-0.0045mg·kg^(-1).Test for recovery was made by standard addition method,giving results in the range of 94.2%-103%,with RSDs(n=6)of the determined values all less than 5.0%.

关 键 词：全自动凝胶渗透色谱法 气相色谱-串联质谱法 有机磷类杀虫剂 茄果类蔬菜 

分 类 号：O657.63[理学—分析化学]