Objective To establish a method for determination of glyphosate,glufosinate and aminomethyl residues in water and foods by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS).Methods The samples were extracted by pure water vortex with ultrasound,and defatted with dichloromethane,then purified by C18 dispersive solid phase extraction column.Purified liquid (water) was adjusted pH by phosphate saline buffer and added 9-fluorene methyl chloroform (FMOC-C1) acetone solution for derivatization for 2 h at least.Derived compounds were filtered through 0.22 μm millipore membrane.The sample extract was separated by CAPCELLCORE C18 column with 5 mmol/L ammonium acetate-acetronitrile as mobile phase for gradient elution,and then identified by electrospray ionization (ESI) in negative mode and multiple reaction monitoring mode,and quantified with external standard method.Results The method showed good linear relationships in the range of 0.5～40 μg/L for glyphosate,glufosinate and aminomethyl with the correlation coefficients ＞ 0.999.The limits of quantitation (LOQ) were 0.5 μg/kg.The average recovery rates spiked at levels of 0.5,5.0 and 20 μg/kg were 70.1％～104.1％ with the relative standard deviations of 0.6％～8.9％ (n=6).Conclusion This method has rapid analysis speed,good purification effect,low impurity interference,high recovery rate and good repeatability,which is suitable for the determination of glyphosate,glufosinate and aminomethyl residues in water and foods.

目的 建立食品中6种工业染料的QuEChER前处理高效液相色谱-串联质谱同时测定方法.方法 均匀样品用水分散溶解后,加乙腈提取,经改进的QuEChERS方法净化,0.22 μm微孔滤膜过滤,用0.1％甲酸-5mmol/L乙酸铵溶液和乙腈为流动相梯度洗脱,C18柱分离,分别在电喷雾正、负离子模式下以多反应监测方式检测,外标法定量.结果 结果表明,6种工业染料在0.5～40 μg/L浓度范围内与其呈良好的线性关系(r＞0.999),检出限为1.0～2.0 μg/kg,在添加水平为1.0、5.0、20μg/kg时,平均回收率为76.1％～114.8％,相对标准偏差(RSD)为2.0％～9.7％(n=6).结论 该方法分析速度快,灵敏可靠,重复性好,适用于调味品、豆制品、卤肉制品、红糖等食品中6种工业染料的测定.