正相硅胶/选择洗脱-气相色谱法、液相色谱-质谱法检测食品中甲胺磷残留及其作用机理研究  

Determination of Residual Methamidophos in Various Food by Solid Phase Extraction with Gas Chromatography,Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry and its Effect Mechanism Study

作　　者：苏建峰 张金虎 林永辉[3] 梁震[1,3] 刘建军 

机构地区：[1]福建华日食品安全检测有限公司,福州350015 [2]福清出入境检验检疫局,福清350300 [3]福建出入境检验检疫局,福州350001 [4]中国检验认证集团福建有限公司,福州350001

出　　处：《分析化学》2009年第10期1426-1432,共7页Chinese Journal of Analytical Chemistry

基　　金：福建出入境检验检疫局科技计划(No.FK2008-14)资助项目

摘　　要：以正相硅胶/选择洗脱为核心,建立了一种适用于各种复杂基质食品中甲胺磷残留分析的前处理方法。样品用无水Na2SO4配合乙酸乙酯均质研磨,超声波辅助提取,提取液经PSA粉末分散固相萃取和LC-Si柱单一溶剂选择洗脱净化后,供气相色谱仪(GC)和超高效液相色谱-串联质谱仪(UPLC-MS/MS)分析。气相色谱采用火焰光度检测器(FPD),液相色谱-质谱联用采用电喷雾正离子方式(ESI+),T3键合技术(HSST3)和亲水作用(HILIC)超高效液相色谱柱分离,外标法定量。方法简便、快速,通过优化前处理和上机条件,在最优条件下进行测试,气相色谱法、液相色谱-质谱联用法的定量下限(S/N≥10)为0.0007～0.006mg/kg,回收率分别为73%～90%,81%～96%,相对标准偏差分别为2.4%～6.1%,5.2%～10.8%。并对选择洗脱净化过程中的作用机理进行了研究。A new pretreatment method was reported that residual methamidophos in various food was pretreated quickly by normal phase silica/selective elution technique.The results were determined by gas chromatography and ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）.The compounds were extracted from homogenized tissue using ethyl acetate and sodium sulfate assisted by ultrasonication.The supernatants were purified by solid phase extraction powder and LC-Si column prior to GC and UPLC-MS/MS analysis.Determinations were performed by using electrospary ionization mode,and the residual pesticide was separated by HSS T3 and HILIC columns in UPLC-MS/MS method.Then external standard method was used in the quantification.The methods were convenient and rapid.Under the optimal conditions,the detection limits for the GC and UPLC-MS/MS methods（S/N≥10） of pesticide were 0.0007-0.006 mg/kg.The tests for recovery were carried by addition of standard at concentration of 0.0025-0.2 mg/kg,the results of GC and UPLC-MS/MS methods were 73%-90% and 81%-96%,while the relative standard deviations were 2.4%-6.1% and 5.2%-10.8% respectively.The effect mechanism of selective elution was also studied.

关 键 词：气相色谱法 超高效液相色谱-串联质谱法 T3键合技术色谱 残留分析 甲胺磷 

分 类 号：TS207.5[轻工技术与工程—食品科学]