液相色谱-串联质谱法检测食品中托曲珠利及其残留标志物

Determination of Toltrazuril and Its Residues in Food by Liquid Chromatography Tandem Mass Spectrometry

目的:建立一种托曲珠利及其残留标志物的液相色谱-串联质谱(HPLC-MS/MS)检测方法。方法:样品经30%乙腈水(含0.5%甲酸)溶液提取,过HLB固相萃取柱净化。采用5 mmol·L^(-1)乙酸铵水溶液和乙腈作为流动相进行梯度洗脱,负离子扫描(ESI-)、多离子检测模式(MRM)对托曲珠利及其残留标志物的定量离子和定性离子进行监测。结果:本方法在7 min内完成托曲珠利及其残留标志物分离分析。托曲珠利及其残留标志物在1μg·kg^(-1)、5μg·kg^(-1)和10μg·kg^(-1)添加水平的回收率为73.4%~104.7%,RSD小于9.2%(n=7),方法定量限为5μg·kg^(-1)。结论:该方法快速、准确、灵敏,适合测定托曲珠利及其残留标志物。

Objective:To establish a HPLC-MS/MS method for the determination of Toltrazuril and its residues.Methods:The sample was extracted with 30% acetonitrile water(containing 0.5% formic acid)and purified by HLB solid phase extraction column.5 mmol·L^(-1) ammonium acetate aqueous solution and acetonitrile were used as mobile phase for gradient elution.The quantitative and qualitative ions of Toltrazuril and its residual markers were monitored by negative ion scanning(ESI-)and multi ion detection mode(MRM).Results:The separation and analysis of Toltrazuril and its residual markers were completed within 7 min.Toltrazuril and its residual markers were detected at 1μg·kg^(-1),5μg·kg^(-1) and 10μg·kg^(-1).The recoveries were 73.4%~104.7% with RSD less than 9.2%(n=7)and the limit of quantitation was 5μg·kg^(-1).Conclusion:The method is rapid,accurate,sensitive and suitable for the determination of Toltrazuril and its residual markers.