基质分散固相萃取-超高效液相色谱串联质谱法同时测定食品中10种杀菌剂和4种杀虫剂  

Determination of 10 kinds of fungicides and 4 kinds of pesticides in food by matrix dispersive solid phase extraction and UPLC-MS/MS

作　　者：和佳鸳 张春玲[1] 蒲彦利[1] 曹杰[1] 王红波 徐虹[1] HE Jia yuan;ZHANG Chun ling;PU Yan li;CAO Jie;Wang Hong bo;XU Hong(Zhenjiang Municipal Center for Disease Control and Prevention, Zhenjiang 212000,China)

机构地区：[1]江苏省镇江市疾病预防控制中心,镇江212000

出　　处：《江苏预防医学》2017年第6期614-618,共5页Jiangsu Journal of Preventive Medicine

摘　　要：目的建立同时测定蔬菜、水果及茶叶中10种杀菌剂和4种杀虫剂的超高效液相色谱串联质谱(UPLC-MS/MS)法。方法样品经乙腈匀浆、饱和氯化钠盐析、无水硫酸镁脱水、离心、固相吸附剂净化后,进液相色谱-质谱系统分析,外标法定量。色谱柱采用WATERS BEH C18柱(2.1mm×100mm,1.7μm);流动相为乙腈-0.1%甲酸,进行梯度洗脱;质谱采用电喷雾离子源,在正离子多反应监测模式下进行检测。结果 14种目标化合物在一定范围内线性关系良好(相关系数r>0.99);检测限(LOD)和定量限(LOQ)分别为3×10^(-5)~3×10^(-3) mg/kg和1×10^(-4)~1×10^(-2)mg/kg;低、中、高浓度准确度分别为91.9%~117.0%、95.3%~111.0%、85.0%~105.0%,精密度(RSD)分别为1.5%~7.0%、0.9%~7.7%、1.0%~6.4%;回收率为80.9~112.0%。结论建立的方法简便、灵敏、准确、稳定,适用于蔬菜、水果及茶叶中10种杀菌剂和4种杀虫剂的同时测定。ObjectiveTo establish an UPLC MS/MS method for determination of10kinds of fungicides and4kinds of pesticides in fruit,vegetables and teas MethodsThe samples were homogenated by acetonitrile,salted out by saturated sodium chloride,dehydrated by anhydrous magnesium sulfate,centrifuged and cleaned up by solid phase adsorbent,and then analyzed by LC MS/MS;external standard method was used for quantitative analysis The WATERS BEH C18column(21mm×100mm,17μm)was selected as separation column;the mobile phase was acetonitrile01%formic acid mixture with gradient elution The mass spectrometry employed electrospray ion source,the positive ions multiple reaction monitoring mode was used for determination Results14target compounds had good linear relationship in certain concentration range(r>099)Limits of detection(LODs)and limits of quantitation(LOQs)were3×10-5-3×10-3mg/kg and1×10-4-1×10-2mg/kg,respectively The accuracy of the method for low,medium and high concentration were919%-1170%,953%-1110%,850%-1050%,respectively;the RSDs were15%-70%,09%-77%,10%-64%,respectively;the recovery rates were809%-1120%ConclusionThe established method is simple,sensitive,accurate and stable which could meet the monitoring requirements of simultaneous determination of10kinds of fungicides and4kinds of pesticides in fruits,vegetables and teas.

关 键 词：超高效液相色谱串联质谱法 基质分散固相萃取 杀菌剂 杀虫剂 

分 类 号：R917[医药卫生—药物分析学]