Determination of Five Macrolide Antibiotic Residues in Raw Milk Using Liquid Chromatography−Electrospray Ionization Tandem Mass Spectrometry
- 23 March 2006
- journal article
- Published by American Chemical Society (ACS) in Journal of Agricultural and Food Chemistry
- Vol. 54 (8), 2873-2880
- https://doi.org/10.1021/jf060068j
Abstract
A confirmatory method using liquid chromatography-electrospray ionization tandem mass spectrometry for determination of five macrolide antibiotics including spiramycin, tilmicosin, oleandomycin, erythromycin, and tylosin in raw milk is presented. Macrolides were extracted from raw milk by acetonitrile, and sample extracts were further cleaned up using solid-phase extraction cartridges. Data acquisition was achieved using multiple reaction monitoring, that is, two transitions, to provide a high degree of sensitivity and specificity. Matrix-matched standard calibration curves with the use of roxithromycin as an internal standard were utilized to achieve the best accuracy of the method. Both a conventional validation procedure and a designed experiment were applied to study the accuracy and precision of the method. The measurement uncertainty arising from accuracy and precision was estimated. The method accuracy, expressed as a percentage of overall recovery, was approximately 100%, and its intermediate precision was or = 3:1) of five macrolides were <0.3 microg/kg.Keywords
This publication has 14 references indexed in Scilit:
- Analysis of erythromycin and benzoylperoxide in topical gels by liquid chromatographyJournal of Chromatography B, 2003
- Effect of non-significant proportional bias in the final measurement uncertaintyThe Analyst, 2003
- Residue analysis of macrolides in poultry muscle by liquid chromatography–electrospray mass spectrometryJournal of Chromatography A, 2002
- Linear regression for calibration lines revisited: weighting schemes for bioanalytical methodsJournal of Chromatography B, 2002
- Analysis of erythromycin and oleandomycin residues in food by high-performance liquid chromatography with fluorometric detectionFood Additives & Contaminants, 2002
- Determination of tylosin residues in different animal tissues by high performance liquid chromatographyJournal of Chromatography B, 2002
- Measurement uncertainty in analytical methods in which trueness is assessed from recovery assaysAnalytica Chimica Acta, 2001
- Identification and quantification of five macrolide antibiotics in several tissues, eggs and milk by liquid chromatography–electrospray tandem mass spectrometryJournal of Chromatography B: Biomedical Sciences and Applications, 2001
- Nested designs in ruggedness testingJournal of Pharmaceutical and Biomedical Analysis, 1999
- Interlaboratory Variability in Trace Element AnalysisAnalytical Chemistry, 1985