超高效液相色谱-串联质谱法测定动物源性食品中9种苯并咪唑类药物残留

Determination of benzimidazoles in Animal-derived Foods by ultra performance liquid chromatography-tandem mass spectrometry

采用超高效液相色谱-串联质谱法(UPLC-MS/MS),建立了测定动物源性食品中9种苯并咪唑类药物残留的方法。样品经乙腈提取,以HLB固相萃取小柱净化,净化液浓缩处理后采用Waters ACQUITY UPLCTM BEH C18柱色谱柱分离,乙腈-0.1%甲酸水溶液为流动相进行梯度洗脱,采用电喷雾正离子模式,多反应监测(MRM)模式下进行检测。9种苯并咪唑类药物在0.20~20 ng/mL范围内线性良好,相关系数(r2)均大于0.99;在空白样品基质中进行3个不同浓度水平的加标实验,平均回收率为82.5%~108%,相对标准偏差在1.8%~7.1%之间(n=6),方法检出限均低于0.1μg/kg。该方法灵敏、准确,具有良好的重复性和稳定性,可用于动物源性食品中苯并咪唑类药物残留的检测。

A method was developed for the simultaneous determination of 9 benzimildazoles residues in animal derived foods by ultra performance liquid chromatography-tandem mass spectrometry((UPLC-MS/MS).The samples were extract⁃ed with acetonitrile,purified with a HLB solid-phase extraction cartridge,chromatographic separation was performed on a Waters ACQUITY UPLCTM BEH C18 chromatographic column using 0.1%formic acid aqueous solution-acetonitrile as the mobile phase under the electrospray ionization mode,analyzed in multiple reaction monitoring(MRM)mode.A calibra⁃tion curve ranging from 0.20-20 ng/mL was established for 9 kinds of benzimildazoles residues,and the correlation coeffi⁃cient(r2)were all greater than 0.99;the spiked experiments at 3 kinds of different concentration levels in the blank sample matrix were performed,and the average recoveries were between 82.5%and 108%,the relative standard deviations were 1.8%-7.1%(n=6),the detection limits were lower than 0.1μg/kg.The method was sensitive,accurate,has good repeatabili⁃ty and stability,and it can be used for the detection of benzimidazoles residues in animal derived foods.