高效液相色谱-串联质谱法测定动物源性食品中20种磺酰脲类除草剂残留

Determination of 20 Sulfonylurea Herbicides Residues in Animal Origin Foods by High Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了动物源性食品中20种磺酰脲类除草剂多残留的分析方法。样品经乙腈均质提取2次,经Waters Oasis HLB固相萃取小柱净化后,在高效液相色谱-电喷雾串联质谱仪多反应监测模式下测定,采用质谱法定性,外标法定量。除草剂采用Eclipse AAA色谱柱,以甲醇和0.1%乙酸溶液为流动相,在梯度洗脱条件下可以得到很好地分离。在6种动物源性食品中分别添加低、中、高3个浓度水平的20种磺酰脲类除草剂,平均回收率为66.07%～112.07%;相对标准偏差为0.7%～19.4%;20种磺酰脲药物在6种动物源性食品中的检出限为0.5～2.5μg/kg。本方法操作简单、净化效果好、灵敏度高,可应用于动物源性食品中20种磺酰脲类药物的实际检测分析。

A method was developed for the determination of 20 sulfonylurea herbicides residues in animal origin foods by high performance liquid chromatographytandem mass spectrometry（LC-MS/MS）.Sulfonylurea herbicides were extracted with acetonitrile and the extract was cleaned up by Waters Oasis HLB solid phase extraction column.Qualitation of the analytes was achieved with multiple reaction monitoring（MRM） and external standard method was used for quantification.The chromatography separation was achieved in gradient mode,on a Eclipse AAA column using methanol and 0.1% acetic acid aqueous solution.The mean recoveries of 20 sulfonylurea herbicides varied from 66.1% to 112.1% in pork,fish,chicken,egg,pork liver and milk samples at three spiked levels.The relative standard deviations（RSDs） were in the range of 0.7%-19.4%.Depending on each herbicide pesticide,the limits of detection were in the range of 0.5-2.5 μg/kg.The proposed method was successfully applied to the determination of sulfonylurea herbicides residues in animal-derived foods.