在线凝胶色谱-气相色谱-串联质谱法测定水果中 甲拌磷和氟虫腈及其代谢产物残留

Determination of phorate, fipronil and their metabolites residues in fruit by online gel permeation chromatography-gas chromatography-tandem mass spectrometry

中文关键词:  QuEChERS方法  在线凝胶渗透色谱-气相色谱-串联质谱法  甲拌磷  氟虫腈  代谢产物  水果

英文关键词:QuEChERS method  online gel permeation chromatography-gas chromatography-tandem mass spectrometry  phorate  fipronil  metabolites  fruit

中文摘要:

      目的 采用在线凝胶渗透色谱-气相色谱-串联质谱(gel permeation chromatography-gas chromatography- tandem mass spectrometry, GPC-GC-MS/MS)法结合QuEChERS方法, 测定水果中甲拌磷和氟虫腈及其代谢产物残留。方法 从样品提取方式、盐析剂、除水剂、净化剂的选择与用量等方面对QuEChERS方法进行优化。样品提取液过滤后, 用在线GPC-GC-MS/MS方法, 在多反应监测模式(multiple reaction monitoring mode, MRM)下进行检测。结果 选择乙腈作为提取溶剂, 氯化钠和无水硫酸镁作为盐析剂和除水剂, N-丙基乙二胺(PSA)、C18填料和无水硫酸镁作为净化剂。在10、40、80 μg/kg 3个加标浓度下, 7种农药在夏黑葡萄、阳山水蜜桃及黄金梨样品中的回收率分别为83.5%~98.7%、80.2%~102.4%和76.5%~109.8%, 检出限分别为0.29~0.85 μg/kg、0.35~0.79 μg/kg和0.21~0.93 μg/kg, 方法的相对标准偏差(relative standard deviation, RSD)为RSD≤9.4%、RSD≤7.6%和RSD≤8.9%。结论 该方法具有分析时间短、样品处理简单、净化效果好、溶剂用量少等优点, 适用于水果中甲拌磷和氟虫腈及其代谢产物残留的快速筛查与常规检测。

英文摘要:

      Objective To determine the residue of phorate, fipronil and their metabolites in fruit by online gel permeation chromatography-gas chromatography-tandem mass spectrometry(GPC-GC-MS/MS) combined with QuEChERS method. Methods The QuEChERS method was optimized from the following aspects: sample extraction method, salting-out agent, water removal agent, cleaning agent and its volume and so on. After filtration, the sample extraction buffer was detected by online GPC-GC-MS/MS with MRM. Results Acetonitrile was selected as the extraction solvent, NaCl was salting-out agent, anhydrous MgSO4 was water removal agent, N-propyl ethylenediamine (PSA), C18 packing and anhydrous MgSO4 were cleaning agent. The recoveries of 7 kinds of pesticides in summer black grape, Yangshan peach and pear samples were 83.5%~98.7%, 80.2%~102.4% and 76.5%~109.8%, respectively, at 3 spiked levels(10, 40, and 80 μg/kg), the limits of detection(LOD) were 0.29~0.85 μg/kg, 0.35~0.79 μg/kg and 0.21~0.93 μg/kg, and the relative standard deviations (RSD) were lower than 9.4%, 7.6% and 8.9%. Conclusion This method is time-saving, simple, easy-pretreating with high purifying efficiency and less solvent consumption, which is suitable for the fast screening and detection of phorate, fipronil and their metabolites residues in fruit.