| Title | Fully Automated Analysis of beta-Lactams in Bovine Milk by Online Solid Phase Extraction-Liquid Chromatography-Electrospray-Tandem Mass Spectrometry. | | Author(s) | Kantiani L, Farré M, Sibum M, Postigo C, López de Alda M, Barceló D | | Institution | Department of Environmental Chemistry, IDAEA-CSIC, c/Jordi Girona 18-26, 08034, Barcelona, Spain, Spark Holland B.V., P.O. Box 388, 7800 AJ Emmen, The Netherlands, and Catalan Institute for Water Research (ICRA), Parc Cientific i Tecnologic de la Universitat de Girona, Edifici Jaume Casademont, Porta A, Planta 1 - Despatx 13C/ Pic de Peguera, 15, E-17003 Girona, Spain. | | Source | Anal Chem 2009 Apr 29. | | Abstract | A fully automated method for the detection of beta-lactam antibiotics, including six penicillins (amoxicillin, ampicillin, cloxacillin, dicloxacillin, oxacillin, and penicillin G) and four cephalosporins (cefazolin, ceftiofur, cefoperazone, and cefalexin) in bovine milk samples has been developed. The outlined method is based on online solid-phase extraction-liquid chromatography/electrospray-tandem mass spectrometry (SPE-LC/ESI-MS-MS). Target compounds were concentrated from 500 muL of centrifuged milk samples using an online SPE procedure with C18 HD cartridges. Target analytes were eluted with a gradient mobile phase (water + 0.1% formic acid/methanol + 0.1% formic acid) at a flow rate of 0.7 mL/min. Chromatographic separation was achieved within 10 min using a C-12 reversed phase analytical column. For unequivocal identification and confirmation, two multiple reaction monitoring (MRM) transitions were acquired for each analyte in the positive electrospray ionization mode (ESI(+)). Method limits of detection (LODs) in milk were well below the maximum residue limits (MRLs) set by the European Union for all compounds. Limits of quantification in milk were between 0.09 ng/mL and 1.44 ng/mL. The developed method was validated according to EU's requirements, and accuracy results ranged from 80 to 116%. Finally, the method was applied to the analysis of twenty real samples previously screened by the inhibition of microbial growth test Eclipse 100. This new developed method offers high sensitivity and accuracy of results, minimum sample pre-treatment, and uses for the first time an automated online SPE offering a high throughput analysis. Because of all these characteristics, the proposed method is applicable and could be deemed necessary within the field of food control and safety. | | Language | ENG | | Pub Type(s) | JOURNAL ARTICLE
| | PubMed ID | 19402673 |
|
