Multi-class, multi residue method for determination of penicillins, cephalosporins and quinolones in cow milk and validation in accordance with Commission Decision 2002/657/E C

Amatya, Rameshwari

http://hdl.handle.net/10400.1/10746

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Authors

Amatya, Rameshwari

Advisor(s)

Torralbo, José Barbosa

Bueno, Dolores Barrón

Cavaco, Isabel Maria Palma Antunes

Abstract(s)

The method was developed to determine simultaneously 19 drugs of three classes (seven Penicillins and Cephalosporins, and five Quinolones) regulated by European legislation 2377/90/EC in cow milk using LC-MS/MS. To make the sample preparation as simple as possible deproteinization step using organic solvent was eliminated. SPE clean up and concentration was done using OASIS HLB cartridge. The separation of 19 antibiotics was achieved in 11 minutes using C8 column with gradient elution. MS data was acquired on MRM mode with two transitions for each compound. Validation procedure was conducted based on European directive 2002/657/EC. 89% of drugs presented recoveries higher than 65 % with exception of AMOX (57%) and DAN (38 %). Repeatability values expressed as relative standard deviation, (RSDs) were not more than 15 %. LODs values ranged from 0.03 (NAFC) to 0.5 μg/kg (PER) and LOQs from 0.1 (NAFC, PENG, CIP, DAN, and ENR) to 1.25 μg/kg (PER). The method was applied to 49 real samples. 37% of the sample was found to be non-compliant with an error probability of 􀉴. Of all samples analysed, 14 % of samples contained AMOX and 16 % contained PENG. AMOX and PENG was the most common residue found in milk sample.