固相萃取-液相色谱串联质谱法测定牛肉中多种磺胺类药物残留量

Determination of Sulfonamide Residues in Beef by Solid Phase Extraction-Liquid Chromatography-Tandem Mass Spectrometry

目的:建立牛肉中多种磺胺类药物残留量的检测方法。方法:处理均质后的牛肉,用乙酸乙酯提取出目标物,用HLB小柱净化,氮吹,复溶。以0.1%的甲酸甲醇与0.1%的甲酸水溶液为流动相进行梯度洗脱,经T_(3)色谱柱进行分离,采用离子源为电喷雾离子源,扫描方式为正离子扫描,检测模式为多反应监测,外标法定量。结果:18种磺胺在2~200 ng·mL^(-1)线性关系良好(r>0.996),方法的检出限为2μg·kg^(-1),定量限为10μg·kg^(-1),加标回收率为64.87%~105.00%,相对标准偏差为1.6%~6.8%。结论:本方法灵敏、准确,适用于牛肉中18种磺胺类药物的检测。

Objective:To establish a method for the determination of sulfonamides residues in beef.Method:The homogenized beef was treated,the target was extracted with ethyl acetate,purified by HLB column,nitrogen blowing,and redissolved.0.1%formic acid methanol and 0.1%formic acid aqueous solution were used as mobile phase for gradient elution,and separated by T_(3) column.Ion source was used as electrospray ion source,scanning mode was positive ion scan,detection mode was multi-reaction monitoring,and quantitative method was external standard method.Result:The internal linear relationship of 18 sulfonamides was good(r>0.996)in the range of 2~200 ng·mL^(-1). The limits of detection and quantification were 2μg·kg^(-1) and 10μg·kg^(-1).The recoveries were 64.87%~105.00%and the relative standard deviations were 1.6%~6.8%.Conclusion:The method is sensitive,accurate and suitable for the detection of 18 sulfonamides in beef.