改良的QuEChERS-超高液相色谱-三重四极杆串联质谱法测定水果中草甘膦、草铵膦及氨基甲磷酸残留量  

Modified QuEChERS-ultra-performance liquid chromatography-tandem mass spectrometry method for the determination of glyphosate,glufosinate and aminomethyl phosphonic acid residues in fruits

作　　者：张文 闫君 赵波 张新中 张婕 陈婷 ZHANG Wen;YAN Jun;ZHAO Bo;ZHANG Xinzhong;ZHANG Jie;CHEN Ting(Gansu Engineering Research Center for Monitoring Exogenous Harmful Residues in Traditional Chinese Medicines,Key Laboratory of Pesticide and Veterinary Drug Monitoring for State Market Regulation,Lanzhou Institute for Food and Drug Inspection and Testing,Lanzhou 730050,China)

机构地区：[1]兰州市食品药品检验检测研究院,国家市场监管重点实验室(食品中农药兽药残留监控),甘肃省种植中药材外源性污染物监测工程研究中心,兰州730050

出　　处：《分析试验室》2025年第4期573-578,共6页Chinese Journal of Analysis Laboratory

基　　金：甘肃省市场监督管理局科技计划项目(SSCJG-SP-A202309);国家市场监督管理总局科技计划项目(2022MK126,2021MK110)资助。

摘　　要：建立了改良的QuEChERS-超高液相色谱-三重四极杆串联质谱法(UPLC-MS/MS)检测水果中草甘膦(GLY)、草铵膦(GLUF)及氨甲基膦酸(AMPA)的残留量。样品采用0.5%甲酸水溶液提取,50 mg石墨化炭黑(GCB)、30 mg N-丙基乙二胺(PSA)和50 mg十八烷基键合硅胶(C18)净化,经9-芴基甲基氯甲酸酯(FMOC-Cl)常温下衍生1 h,正离子多反应监测(MRM)模式,外标法定量。3种目标物具有较好的线性关系,相关系数(r)均大于0.999,在0.05,0.15,0.30 mg/kg 3个梯度加标量下,GLY,GLUF和AMPA的回收率为73.8%~94.3%,相对标准偏差为3.1%~7.6%,检出限分别为9.950,13.64,6.850μg/kg,定量限分别为29.85,40.92,20.55μg/kg。该方法适用于水果中GLY,GLUF和AMPA残留的批量检测。An analytical method was developed for the simultaneous determination of glyphosate(GLY),glufosinate(GLUF)and aminomethyl phosphonic acid(AMPA)residues in fruits by ultra-performance liquid chromatographytandem mass spectrometry(UPLC-MS/MS)coupled with a modified QuEChERS method.The samples were extracted with 0.5%formic acid aqueous solution,purified by 50 mg graphitized carbon black(GCB),30 mg N-propyl ethylenediamine(PSA)and 50 mg C18,and derived using 9-fluorenylmethyl chlorformate(FMOC-Cl)in borate buffer solution at room temperature for 1 h.The derivatives of GLY,GLUF and AMPA were detected with positive electrospray ionization-mass spectrometry(ESI-MS/MS)in the multiple reaction monitoring(MRM)mode and quantified by external standard method.The correlation coefficients(r)of the three substances were all greater than 0.999.At spiked levels of 0.05,0.20 and 0.50 mg/kg,the recoveries of GLY,GLUF and AMPA were 73.8%-94.3%,with the relative standard deviations of 3.1%-7.6%.The limits of detection were 9.950,13.64,and 6.850μg/kg,and the limits of quantification were 29.85,40.92,and 20.55μg/kg,respectively.This method is suitable for the simultaneous detection of GLY,GLUF and AMPA residues in fruits.

关 键 词：超高效液相色谱-串联质谱法 草甘膦 草铵膦 氨基甲磷酸 水果 

分 类 号：TS207[轻工技术与工程—食品科学] O657[轻工技术与工程—食品科学与工程]