超高效液相色谱-串联质谱法测定鸡蛋中沙拉沙星残留的研究

Determination of salafloxacin residues in eggs by ultra performance liquid chromatography-tandem mass spectrometry

关键词:  沙拉沙星  鸡蛋  残留检测  液相色谱串联质谱法

Key words:  Sarafloxacin  egg  residue detection  LC-MS/MS

摘要:

建立了鸡蛋中沙拉沙星残留检测的液相色谱-串联质谱法。样品经1 mol/L磷酸和乙腈提取后，饱和正己烷除脂净化，以0.1%甲酸溶液和乙腈为流动相，液相色谱-串联质谱法测定，内标法定量。试验结果表明：沙拉沙星在1~25 ng/mL浓度范围内线性关系良好，相关系数r大于0.999。沙拉沙星在全鸡蛋及其蛋清、蛋黄中的检测限均为0.5 μg/kg，定量限为1 μg/kg。沙拉沙星在1 μg/kg、10 μg/kg和20 μg/kg浓度添加水平内的平均回收率范围为97.0%~105.4% ，批内、批间相对标准偏差在1.3%~10.3%范围之间。本方法适用于全鸡蛋及其蛋清、蛋黄中沙拉沙星残留量的测定。

Abstract:

A liquid chromatography-tandem mass spectrometry (LC-MS) method was developed for the determination of salafloxacin residues in eggs. The sample was extracted with 1 mol/L phosphoric acid and acetonitrile, purified by saturated hexane, and determined by liquid chromatography-tandem mass spectrometry with 0.1% formic acid solution and acetonitrile as mobile phases, and quantified by internal standard method. The test results showed that the linearity of salafloxacin was good in the concentration range of 1~25 ng/mL, and the correlation coefficient r ＞0.999.The limits of detection were 0.5 μg/kg and the limits of quantification were 1 μg/kg for salafloxacin in whole eggs, albumens and yolks. The average recoveries of salafloxacin at 1 μg/kg, 10 μg/kg and 20 μg/kg spiked levels ranged from 97.0% to 105.4% with the relative standard deviations (RSDs) of 1.3%-10.3% within and between batches. This method is suitable for the determination of salafloxacin residues in whole eggs, albumens and yolks.