基于QuEChERS方法的血液中30种农药的气相色谱-质谱快速检测法  

Determination of 30 pesticides in blood by modified QuEChERS coupled with gas chromatography-mass spectrometry

作　　者：周闰[1] 吴林林 刘文卫[1] ZHOU Run;WU Lin-lin;LIU Wen-wei(Center for Disease Control and Prevention of Wuxi,Wuxi,Jiangsu 214023,China)

机构地区：[1]无锡市疾病预防控制中心

出　　处：《现代预防医学》2019年第13期2448-2454,共7页Modern Preventive Medicine

基　　金：无锡市“科教强卫工程”项目《公共卫生突发事件应急监测实验室》(CXPT(SYS)002)

摘　　要：目的建立血液中30种有机氯及菊酯类农药的气相色谱-质谱检测方法。方法取0.50ml全血,加入乙腈沉淀蛋白,并超声提取待测农药,经QuEChERS法净化后,样液经2根串联的HP-5MS(15m×0.25mm×0.25μm)毛细管柱分离,质谱检测。结果各农药浓度在0.005~2.0mg/L范围内线性关系良好,相关系数均大于0.995,检出限(LOD)为0.002~0.004mg/L,定量限(LOQ)为0.005~0.010mg/L,回收率为60.42%~99.88%,相对标准差为2.84%~21.46%。结论该方法操作简便、快速、灵敏、稳定性好,适合于血液样品中30种农药残留的检测。Objective To develop a method for the determination of 30 pesticides in blood by Gas Chromatography-Mass Spectrometry(GC-MS).Methods 0.5 ml whole blood was taken and acetonitrile was added to precipitate protein and the pesticide to be tested was ultrasonically extracted.After purification by QuEChERS method,the separation was accomplished with two DB-5MS(15 m×0.25 mm×0.25μm)capillary columns connected in series and the detection was conducted by the mass spectrometer.Results The linear relationship of the method was in the range of 0.005 to 2.0 mg/L.The limits of detection(LODs)of the method were in the range of 0.002~0.004 mg/L,and the relative standard deviation was 2.84%-21.46%.The recovery rate was between 60.42%and 99.88%.Conclusion The method is rapid,sensitive and selective,it can be applied to rapid detection of 30 pesticides residues in the blood.

关 键 词：有机氯农药 拟除虫菊酯农药 血液 气相色谱-质谱法 

分 类 号：R115[医药卫生—公共卫生与预防医学]