Determination of five macrolide antibiotic residues in eggs using liquid chromatography/electrospray ionization tandem mass spectrometry.
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.
Wang
Jian
J
Calgary Laboratory, Canadian Food Inspection Agency, 3650 36th Street N.W., Calgary, Alberta, T2L 2L1, Canada. wangj@inspection.gc.ca
Leung
Daniel
D
Butterworth
Fred
F
D000900:Anti-Bacterial Agents / Q000032:analysis*; D002853:Chromatography, Liquid; D004531:Eggs / Q000032:analysis*; D004917:Erythromycin / Q000032:analysis; D018942:Macrolides / Q000032:analysis*; D013058:Mass Spectrometry; D009827:Oleandomycin / Q000032:analysis; D012680:Sensitivity and Specificity; 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