HPLC-MS联用法测定猪肉组织中5种磺胺类药物的残留

建立一种用高效液相色谱与质谱联用法测定猪肉组织中磺胺类药物残留的方法,该方法检测猪肉中的磺胺类药物快速、准确。样品经2%的醋酸水溶液提取后通过固相萃取柱净化,用甲醇洗脱,吹干,然后用流动相A溶解,用DAD及MS检测器检测。采用AgilentHC-C18(4.6×250mm,5μm)色谱柱,以0.3%甲酸和5%甲醇的水溶液-0.3%甲酸的甲醇溶液为流动相进行梯度洗脱。在添加水平为0.1mg/kg,0.2mg/kg,0.5mg/kg时,对于不同的药物,回收率范围为55.3%~102.8%,相对标准偏差在0.79%~10.4%之间,方法的最低检出限为0.1~0.5ppb。通过大量的实验结果表明,该方法适用于猪肉组织中磺胺类药物的残留测定。

Determination of 5 sulfonamides in swine tissues by HPLC-MS

A simple and rapid method was developed for the determination of 5 sulfonamides in swine tissues by high performance liquid chromatography tandem mass spectrometry.The proposed method is sensitive and selective.The samples were extracted with 2% acetic acid,purified with solid-phase extraction column,the samples were detected by DAD and MSD.The separation was performed on a Agilent HC-C18(4.6×250mm,5μm) column with a gradient system of water(containing 0.3% for formic acid and 5% methanol)-methanol(containing 0.3% for formic acid) as mobile phases.At spiked levels are 0.1mg/kg,0.2mg/kg,0.5mg/kg,the limits of detection of the method are 0.1~0.5ppb for he various antibiotics and the recoveries of the spike experiment is from 55.3% to 102.8%,precisions are between 0.79%~10.4%.The results showed that the method is suitable for the determination of residues of sulfonamide in swine tissues.