Wang Jian, Leung Daniel, Butterworth Fred
Calgary Laboratory, Canadian Food Inspection Agency, 3650 36th Street N.W., Calgary, Alberta, T2L 2L1, Canada.
J Agric Food Chem. 2005 Mar 23;53(6):1857-65. doi: 10.1021/jf048414p.
A method using liquid chromatography electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) for the determination of trace levels of five macrolide antibiotics (spiramycin, tilmicosin, oleandomycin, erythromycin, and tylosin) in eggs is presented. Data acquisition under MS/MS was achieved by applying multiple reaction monitoring (MRM) of two or three fragment ion transitions to provide a high degree of sensitivity and specificity for both quantification and confirmation. Matrix-matched standard calibration curves were used to achieve the best accuracy of the method. A fully nested experimental design was used to study the measurement uncertainty arising from intermediate precision and trueness or proportional bias. The overall recoveries, that is, those determined by the nested experiments, of spiramycin, tilmicosin, oleandomycin, erythromycin, and tylosin at fortified levels of 60, 100, 200, and 300 microg/kg were 96.8, 98.2, 98.3, 98.8, and 95.4%, respectively. The LC/ESI-MS/MS method detection limits (S/N > or = 3:1) of five macrolides were <1.0 microg/kg.
本文介绍了一种采用液相色谱-电喷雾电离串联质谱法（LC/ESI-MS/MS）测定鸡蛋中痕量水平的5种大环内酯类抗生素（螺旋霉素、替米考星、竹桃霉素、红霉素和泰乐菌素）的方法。在MS/MS模式下的数据采集通过对两个或三个碎片离子跃迁进行多反应监测（MRM）来实现，从而为定量和确证提供高度的灵敏度和特异性。采用基质匹配标准校准曲线以实现该方法的最佳准确度。使用完全嵌套实验设计来研究由中间精密度以及真实性或比例偏差产生的测量不确定度。螺旋霉素、替米考星、竹桃霉素、红霉素和泰乐菌素在60、100、200和300μg/kg加标水平下的总回收率（即通过嵌套实验测定的回收率）分别为96.8%、98.2%、98.3%、98.8%和95.4%。5种大环内酯类化合物的LC/ESI-MS/MS方法检测限（S/N≥3:1）均<1.0μg/kg。
