超高效液相色谱-质谱联用法快速测定蔬菜中氰氟虫腙残留  

Determination of Metafl umizone Residues in Different of Vegetables by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：占绣萍[1] 陈建波[1] 马琳[1] 赵莉[1] 姜皞 

机构地区：[1]上海市农业技术推广服务中心,上海201103 [2]崇明县食用农产品监测中心,上海202150

出　　处：《农药》2014年第7期497-499,511,共4页Agrochemicals

基　　金：上海市地方标准制修订项目(沪质技监标[2013]301号-55)

摘　　要：[目的]建立一种超高效液相色谱一质谱联用法测定不同品种蔬菜中氰氟虫腙的残留量。【方法】蔬菜样品用乙腈提取，分散固相萃取法净化，液相色谱一质谱法进行定性和定量。以Poroshell 120 Eclipse plus C18柱为分析柱，甲醇和5mmol／L乙酸铵水溶液为流动相进行梯度洗脱，在电喷雾负离子多反应监测模式下进行检测。【结果】氰氟虫腙在0．005—0．5mg／L范围内线性关系良好，线性相关系数为0．9989。在0．01、0．05、0．25mg／kg三个质量分数水平进行了添加回收试验，在6个不同品种的蔬菜中氰氟虫腙平均回收率为73．6％-110．9％，相对标准偏差为0．5％-7．4％，方法的最低检测质量分数为0．01mg／kg。【结论】该方法操作简单、快速、准确，可用于不同种类蔬菜中氰氟虫腙的日常检测。[Aims] A ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS） method was developed for the determination of metaflumizone in vegetables. [Methods] After the residues of sample were extracted with acetonitrile, the samples were purified with dispersive solid-phase extraction method. The separation of the analytes was carried out on a Eclipse plus C18 column using the mobile phase of acetonitrile and 5 mmol/L ammonium acetate aqueous solution with gradient elution. The compounds were detected in multiple reaction monitoring （MRM） mode via negative electrospray ionization （ESI）. [Results] The calibration curves were of good linearity in the range of 0.005-0.5 mg/L （r=0.9989）. The limit of quantification of the method was 0.01 mg/kg. The average recoveries were between 73.6-110.9% at three spiked levels （0.01, 0.05, 0.25 mg/kg） with the relative standard deviations （RSDs） in the range of 0.5-7.4%. [Conclusions] The method is simple, rapid and accurate, and could be used for the routine analysis of metaflumizone in different kinds of vegetables.

关 键 词：液相色谱-质谱 氰氟虫腙 残留 蔬菜 

分 类 号：O657.63[理学—分析化学] TS255.7[理学—化学]