Wang Jian
Calgary Laboratory, Canadian Food Inspection Agency, 3650 36th Street N.W., Calgary, Alberta, Canada T2L 2L1.
J Agric Food Chem. 2004 Jan 28;52(2):171-81. doi: 10.1021/jf034823u.
Liquid chromatography-electrospray ionization mass spectrometry methods (LC-ESI-MS and LC-ESI-MS/MS) for the determination of five macrolide antibiotics including spiramycin, tilmicosin, oleandomycin, erythromycin, and tylosin in honey are presented. Macrolides were protonated to form singly and/or doubly charged pseudomolecular ions, depending on their chemical structures, in an electrospray positive ionization mode. 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. The recoveries, that is, determined by LC-ESI-MS/MS, of the five macrolides at fortified levels of 6, 16, 40, and 80 microg/kg ranged from 75.5 to 135.7% in light honey and from 42.1 to 111.0% in dark honey. The ion ratios obtained under MS/MS were key criteria to confirm the identity of macrolides in incurred samples. LC-ESI-MS/MS method detection limits of the five macrolides were <0.1 microg/kg.
介绍了用于测定蜂蜜中螺旋霉素、替米考星、竹桃霉素、红霉素和泰乐菌素这五种大环内酯类抗生素的液相色谱 - 电喷雾电离质谱法（LC - ESI - MS和LC - ESI - MS/MS）。在电喷雾正离子模式下，大环内酯类化合物根据其化学结构被质子化，形成单电荷和/或双电荷的准分子离子。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MS/MS模式下的数据采集，以提供高度的灵敏度和特异性。通过LC - ESI - MS/MS测定，在添加水平为6、16、40和80μg/kg时，这五种大环内酯类化合物在浅色蜂蜜中的回收率为75.5%至135.7%，在深色蜂蜜中的回收率为42.1%至111.0%。在MS/MS模式下获得的离子比率是确认实际样品中大环内酯类化合物身份的关键标准。这五种大环内酯类化合物的LC - ESI - MS/MS方法检测限均<0.1μg/kg。
