engleski

Validation of a multiclass method for the screening and confirmation of 12 antimicrobial groups in muscle

A multiclass method for the screening and confirmation of residues from 12 different drug families has been devoleped. According to CD 2002/657/EC a LC-HRMS method was validated in different muscle species. Acetonitrile was used for extraction, followed by shaking, centrifugation and extract evaportaion. Samples were redissolved in methanol/water mixture (1+4) and centrifuged at 15000 rpm. Optimal chromatography parameters were achieved on a Acquity UPLC HSS-T3 column (1.8 um, 2.1x150 mm) with gradient starting from 100% of 0.1% formic acid to 95% of methanol. Time Of Flight mass spectrometry was used in MS mode collecting all ions uder defined collission energies. Results were obtained using personal database created by targeted scanninig of each analyte. Main criterias used for identification were mass accuracy (ppm), isotopic pattern, fragment confirmation and retention time. 96 samples were analysed at concentration range of interest, in three different days and different coniditions. Calculation of validation parameters were carried out using InterVal Plus software. Precision and trueness were satisfactory for all analytes, what resulted with acceptable CCα and CCβ values. Significant ion supression and ion enhancement was observed in diferent animal species. The validation results demonstrate that the method is suitable for veterinary drug analysis and confirmation of suspect samples.

ntimicrobal drugs ; multiclass method ; validation ; LC-HRMS

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