液相色谱-串联质谱检测水果中杀菌剂及其污染情况调查  

Development of liquid chromatography tandem mass spectrometry for determination of fungicides in fruit and the survey of fungicide pollutions

作　　者：陈丽惠[1] 陈秦秦 蔡伟鹏[1] 贾玉珠[1] 

机构地区：[1]厦门市疾病预防控制中心,厦门361021

出　　处：《分析试验室》2017年第8期961-965,共5页Chinese Journal of Analysis Laboratory

摘　　要：建立了同时检测水果中6种杀菌剂(甲霜灵、嘧霉胺、烯酰吗啉、咪鲜胺、三唑酮、苯醚甲环唑)的分散固相萃取-液相色谱-串联质谱方法。水果样品匀浆后经乙腈提取、Al2O3萃取剂净化后,采用C18色谱柱分离,多反应监测模式(+)进行检测,外标法定量分析。结果表明,在优化条件下,6种杀菌剂在2.5~100 ng/m L之间线性良好(R>0.99)。在0.016,0.040和0.80mg/kg的添加水平下平均回收率为77.0%~110.8%,相对标准偏差(n=3)为0.6%~7.9%,检出限(S/N=3)为0.03~1.0μg/kg。所采集的56份水果样品中6种杀菌剂的总检出率为3.6%~58.9%,其中,以苯醚甲环唑检出率最高。A method was developed for determination of 6 fungicides（ metalaxyl,pyrimethanil,dimethomorph, prochloraz, triadimefon and difenoconazole） in fruit by dispersive solid phase extraction and liquid chromatography tandem mass spectrometry. The fruit sample was extracted by acetonitrile and separated by C18,and then determined on HPLC-MS/MS by using multiple reaction monitoring（ ＋）. Quantification was done by the external standard curves. The standard curves of fungicidesshowed good linear responses in the range of 2. 5 - 100 ng/m L. Recoveries of fungicides were in the range of 77. 0% - 110. 8%,and relative standard deviations were in the range of 0. 6% - 7. 9%at the spiked levels of 0. 016,0. 040 and 0. 80 mg/kg. The limits of detection（ S/N = 3） were in the range of 0. 03 - 1. 0 μg/kg. The total detectable rates of 6 fungicides in 56 samples of fruitswerein the range of 3. 6% - 58. 9%,and the total detectable rate ofdifenoconazole was higher than that of other fungicides.

关 键 词：杀菌剂 分散固相萃取 液相色谱-串联质谱 水果 

分 类 号：TQ450.263[化学工程—农药化工]