Wang Siwei, Zeng Guangfeng, Liu Yanping, Wang Xiaonan, Sun Haibin
Guangdong Provincial Key Laboratory of High Technology for Plant Protection, Institute of Plant Protection, Guangdong Academy of Agricultural Sciences, Guangzhou 510640, China.
Guangdong Inspection and Quarantine Technology Center, Guangzhou 510623, China.
Se Pu. 2019 Jan 8;37(1):93-99. doi: 10.3724/SP.J.1123.2018.08002.
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.
建立了一种高效液相色谱-三重四极杆质谱联用法测定荔枝和香蕉中草铵膦及其代谢物的方法。样品用水超声提取，离心沉淀，经0.22μm微孔滤膜过滤。样品提取物用Extend-C18柱分离，以0.1%氨水-甲醇（9:1，v/v）为流动相进行等度洗脱，采用电喷雾电离负离子模式和多反应监测模式进行定性分析，外标法定量。此外，还对预处理和质谱条件进行了讨论。该方法在1-1000μg/L范围内对草铵膦及其代谢物具有良好的线性关系。荔枝和香蕉样品在50、100、1000μg/kg加标水平下，平均回收率为82.9%-98.6%，相对标准偏差为2.6%-6.3%。方法的检出限为5-10μg/kg。该方法分析速度快，可靠性和灵敏度高，适用于荔枝和香蕉样品中草铵膦及其代谢物的快速测定。
