基于高效液相色谱-三重四极杆质谱技术测定荔枝和香蕉中的草铵膦及3种代谢物

采用高效液相色谱-三重四极杆质谱技术,建立了荔枝和香蕉中草铵膦及3种代谢物的检测分析方法。样品加水超声提取,离心沉淀后进样分析,分析物经Extend-C18色谱柱分离,以0. 1%氨水-甲醇(9∶1,v/v)作为流动相等度洗脱,在电喷雾负离子扫描、多反应监测模式下,外标法定量分析,同时探讨了前处理和仪器分析条件对草铵膦及代谢物的影响效果。结果表明,草铵膦及3种代谢物在1～1 000μg/L范围内,峰面积与质量浓度的线性关系良好;当添加浓度水平在50、100、1 000μg/kg时,草铵膦及代谢物在荔枝和香蕉中的平均回收率为82. 9%～98. 6%,相对标准偏差(RSD)为2. 6%～6. 3%,检出限(LOD)为5～10μg/kg。本方法简化了样品前处理步骤,具有良好的可靠性和灵敏度,适于荔枝和香蕉中草铵膦及其代谢物的快速分析。

Determination of glufosinate-ammonium and its three metabolites in litchi and banana by high performance liquid chromatography coupled with triple quadrupole mass spectrometry

A method was developed for the determination of glufosinate-ammonium and its metabolites in litchi and banana by high performance liquid chromatography coupled with triple quadrupole mass spectrometry. The samples were ultrasound extracted by water, centrifuged to precipitate, and filtered through a 0.22 μm Millipore membrane. The sample extract was separated by an Extend-C18 column with 0.1% ammonia-methanol (9:1, v/v) as mobile phase with an isocratic elution, identified by electrospray ionization in negative and multiple reaction monitoring modes, and quantified with external standard method. Moreover, the pretreatment and mass spectrometry conditions were discussed. The method showed good linear relationship in the range of 1-1000 μg/L for glufosinate-ammonium and its metabolites. The average recoveries ranged from 82.9% to 98.6% with the relative standard deviations of 2.6%-6.3% when the litchi and banana samples were spiked at 50, 100, 1000 μg/kg. The limits of detection were 5-10 μg/kg. The method has rapid analysis speed as well as high reliability and sensitivity, which are suitable for the fast determination of glufosinate-ammonium and its metabolites in litchi and banana samples.