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| 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 | |
| 引用本文： | 苏建峰,张金虎,林永辉,梁震,刘建军.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[J].分析化学,2009,37(10). |
| 作者姓名： | 苏建峰 张金虎 林永辉 梁震 刘建军 |
| 作者单位： | 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. 福建华日食品安全检测有限公司,福州,350015;福建出入境检验检疫局,福州,350001 5. 福建华日食品安全检测有限公司,福州,350015;中国检验认证集团福建有限公司,福州,350001 |
| 基金项目： | 福建出入境检验检疫局科技计划 |
| 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(HSS T3)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0.0007～0.006 mg/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. |
| 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 |
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 |
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| SU Jian-Feng,ZHANG Jin-Hu,LIN Yong-Hui,LIANG Zhen,LIU Jian-Jun.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[J].Chinese Journal of Analytical Chemistry,2009,37(10). | |
| Authors: | SU Jian-Feng ZHANG Jin-Hu LIN Yong-Hui LIANG Zhen LIU Jian-Jun |
| Institution: | SU Jian-Feng1,ZHANG Jin-Hu2,LIN Yong-Hui3,LIANG Zhen1,3,LIU Jian-Jun1,41(Fujian Fairreach Food Safety Testing Co.,Ltd,Fuzhou 350015)2(Fuqing Entry-Exit Inspection and Quarantine Bureau,Fuqing 350300)3(Fujian Entry-Exit Inspection and Quarantine Bureau,Fuzhou 350001)4(China Certification & Inspection Group Fujian Co.,Fuzhou 350001) |
| Abstract: | 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... |
| Keywords: | Gas chromatography ultra performance liquid chromatography-tandem mass spectrometry bonded technique residual determination methamidophos |
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