Determination of five macrolide antibiotic residues in honey by LC-ESI-MS and LC-ESI-MS/MS.
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.
Wang
Jian
J
Calgary Laboratory, Canadian Food Inspection Agency, 3650 36th Street N.W., Calgary, Alberta, Canada T2L 2L1. wangj@inspection.gc.ca
D000900:Anti-Bacterial Agents / Q000032:analysis*; D002853:Chromatography, Liquid; D004917:Erythromycin / Q000032:analysis; D006722:Honey / Q000032:analysis*; D018942:Macrolides / Q000032:analysis*; D009827:Oleandomycin / Q000032:analysis; D015203:Reproducibility of Results; D021241:Spectrometry, Mass, Electrospray Ionization; D015572:Spiramycin / Q000032:analysis; D015645:Tylosin / Q000031:analogs & derivatives* / Q000032:analysis
D000900:Anti-Bacterial Agents; D018942:Macrolides; D004917:Erythromycin; D015572:Spiramycin; D009827:Oleandomycin; C052319:tilmicosin; D015645:Tylosin