多壁碳纳米管分散固相萃取-液质联用技术测定 茶叶中草甘膦、草铵膦、氨甲基膦酸残留量
目的 建立茶叶中草甘膦、草铵膦和氨甲基膦酸残留量的超高效液相色谱串联质谱分析方法。方法 样品经水提取后采用分散固相萃取技术, 以多壁碳纳米管(MWCNTS)和N-丙基乙二胺键合固相吸附剂(PSA)吸附提取液中的杂质, 上清液用9-芴基氯甲酸酯(FMOC-Cl)衍生。衍生物用BEH C18进行分离, 以乙腈-4 mmol乙酸铵水溶液为流动相, 电喷雾正离子模式电离(ESI ), 多反应监测模式检测(MRM), 外标法定量。结果 方法的线性范围是0.1?1 μg/mL, 相关系数大于0.999, 定量限为10 μg/kg, 以绿茶为基质, 三种物质添加水平分别为0.25、0.50、1.00 mg/kg, 回收率范围分别为草甘膦95%~116%, 草铵膦98%~118%, 氨甲基膦酸74%~84%, 精密度均小于6.79%(n=6)。结论 该方法具有简便快速、灵敏度高、准确性强等特点, 适合于测定茶叶中草甘膦、草铵膦和氨甲基膦酸的含量。
Objective An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) analysis method was established for simultaneous determination of glyphosate, glufosinate and aminomethylphonic acid (AMPA) in tea. Methods The sample was extracted with water, and cleaned up by multi-walled carbon nanotubes(MWCNTS)and primary-secondary amine(PSA)as dispersive solid-phase extraction sorbent, then derived using fluorenyl methyl chloroformate(FMOC-Cl). The derivatives were separated by ACQUITY UPLC BEH C18 column, using acetonitrile and 4 mmol/L ammonium acetate as the mobile phase. The identification and quantification of glyphosate, glufosinate and AMPA were carried out by MS/MS in positive electrospray ionization(ESI ) and multiple reaction monitoring(MRM) mode, and the quantification analysis was performed by external standard method. Results The calibration curve showed a good linearity in the range of 0.1?1 μg/mL with the correlation coefficient r2> 0.999. The quantification (LOQ) limits were 10 μg/kg. The average recoveries of glyphosate, glufosinate and AMPA spiked at 0.25, 0.50 mg/kg and 1.00 mg/kg levels in green tea were 95%~116%, 98%~118% and 74%~84%, and the relative standard deviations (RSD, n=6) were lower than 6.79%. Conclusion This method is simple, effective and sensitive, and it is suitable for the determination and confirmation of glyphosate, glufosinate and AMPA in tea.
标题：多壁碳纳米管分散固相萃取-液质联用技术测定 茶叶中草甘膦、草铵膦、氨甲基膦酸残留量
英文标题：Determination of glyphosate, glufosinate and aminomethylphonic acid residues in tea by liquid chromatography-tandem mass spectrometry using multi-walled carbon nanotubes as dispersive solid-phase extraction sorbent
作者：
冯月超 北京市理化分析测试中心,北京市食品安全分析测试工程技术研究中心
马立利 北京市理化分析测试中心,北京市食品安全分析测试工程技术研究中心
贾丽 北京市理化分析测试中心,北京市食品安全分析测试工程技术研究中心
张春梅 北京市理化分析测试中心,北京市食品安全分析测试工程技术研究中心
刘艳 北京市理化分析测试中心,北京市食品安全分析测试工程技术研究中心
范筱京 北京市理化分析测试中心,北京市食品安全分析测试工程技术研究中心
潘灿平 中国农业大学理学院
中文关键词:液质联用,草甘膦,草铵膦,氨甲基磷酸,茶叶,多壁碳纳米管,分散固相萃取,
英文关键词:ultra performance liquid chromatography-tandem mass spectrometry,glyphosate,glufosinate,aminomethylphonic acid,tea,multi-walled carbon nano-tubes,dispersive solid-phase extraction,
发表日期：2014-02-12
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