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NRL Proficiency Study Report

NRL Proficiency Study Report

Lab code of participant

Lab code of participant A B C D E F Table 4. Overview of the samples dispatched to the different participants Performed analysis Screening sulfonamides and macrolides Screening macolides and screening + confirmation sulfonamides Screening and confirmation sulfonamides Screening sulfonamides and macrolides Screening Confirmation 8 Sample Code SM.2010-A-1 SM.2010-A-2 SM.2010-A-3 SM.2010-A-4 SM.2010-A-5 SM.2010-B-1 SM.2010-B-2 SM.2010-B-3 SM.2010-B-4 SM.2010-B-5 SM.2010-C-1 SM.2010-C-2 SM.2010-C-3 SM.2010-C-4 SM.2010-C-5 SM.2010-D-1 SM.2010-D-2 SM.2010-D-3 SM.2010-D-4 SM.2010-D-5 SM.2010-E-1 SM.2010-E-2 SM.2010-E-3 SM.2010-E-4 SM.2010-E-5 SM.2010-F-1 SM.2010-F-2 SM.2010-F-3 SM.2010-F-4 SM.2010-F-5 Expected result Containing sulfadiazine Containing tylosin Containing sulfadiazine containing tylosin Blank Containing tylosin Blank Containing tylosin Containing sulfadiazine Containing sulfadiazine Containing sulfadiazine Containing sulfadiazine Containing for tylosin Blank Containing tylosin Blank Containing sulfadiazine Containing tylosin Containing sulfadiazine Containing tylosin Containing tylosin Containing tylosin Blank Containing sulfadiazine Containing sulfadiazine Blank Containing tylosin Containing tylosin Containing sulfadiazine Containing sulfadiazine

5. Analytical methodologies One participant did not submit their results of the proficiency test (Lab D). Nevertheless the inscription was send to the IPH. Six laboratories participated in this proficiency study. All participants were free to use their proper analytical method to perform the proficiency test. The different methods for screening and confirmatory analysis of macrolides and sulfonamides are summarized in Table 5 and 6, respectively. 5.1. Macrolides For the macrolide analysis, four laboratories participated (Table 5). Three of the laboratories participated for a screening (Lab A, B and E) (Table 4). Laboratory F confirmed the macrolide antibiotics with LC-MS/MS after an extraction with a TRIS buffer and further SPE extraction. Two participants used a microbiological and/or receptor assay to perform a screening of the samples (participants B and E). While laboratory A used rapid acetonitrile extraction followed by evaporation and subsequent UPLC-MS/MS analysis (Lab A). Lab Analysis Table 5. Summary of the used methods for macrolide analysis IS Technique A Screening --- UPLC-MS/MS B Screening --- Premi-test ® Charm II ® Test ELISA kit tylosin 9 Extraction/purification ACN extraction, Centrifugation and Concentration Solvent extraction Protocol Charm Sciences Protocol Tecna S.r.l. C Did not participate in the macrolide analysis D Did not submit their results CCα µg kg -1 CCβ µg kg -1 --- --- / 50 E Screening --- Premi-test ® --- --- --- F Confirmation Roxithromycin LC-MS/MS Extraction TRIS buffer Acidic deproteinisation SPE (OASIS HLB ® ) --- --- --- ≤ 12.5 400 10 123 147

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