液相色谱串联质谱法测定鸡蛋、牛奶和羊奶中泰乐菌素A残留的研究

Determination of Tylosin A Residues in Eggs, Milk and Goat Milk by Liquid Chromatography-Tandem Mass Spectrometry

关键词:  泰乐菌素A  鸡蛋  牛奶  羊奶  残留检测  液相色谱串联质谱法

Key words:  tylosin  egg  milk  goad milk  residue detection  LC-MS/MS

摘要:

建立了鸡蛋、牛奶和羊奶中泰乐菌素A残留的液相色谱-串联质谱法，样品经乙腈提取，Prime HLB固相萃取柱净化，以0.1%甲酸水和乙腈为流动相，液相色谱-串联质谱法测定，内标法定量。试验结果表明：泰乐菌素A在1~100 ng/mL浓度范围内线性关系良好，相关系数r大于0.99。泰乐菌素A在鸡蛋、牛奶和羊奶中的检测限为2 ng/mL，定量限为5 ng/mL。泰乐菌素A在5 ng/g~600 ng/g浓度添加水平内的平均回收率为86.3%~98.5%，批内、批间变异系数在2.7%~10.4%范围之间。本方法适用于鸡蛋、牛奶和羊奶中泰乐菌素A残留的测定。

Abstract:

A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for the determination of tylosin A residues in eggs,milk and goat milk . The samples were extracted by acetonitrile, cleaned up by a Prime HLB solid phase extraction column, and determined by liquid chromatography-tandem mass spectrometry with 0.1% formic acid water and acetonitrile as mobile phases, and quantified by internal standard method. The linearity of tylosin A was good in the concentration range of 1~100 ng/mL with the correlation coefficient r >0.99. The limits of detection were 2 ng/mL and the limits of quantification were 5 ng/mL for tylosin A in eggs, milk and goat milk. The average recoveries of tylosin A ranged from 86.3% to 98.5% at the spiked levels range from 5 ng/g to 600 ng/g. The coefficient of variation within and between batches were in the range of 2.7%~10.4%. This method is suitable for the determination of tylosin A residues in eggs,milk and goat milk.