<p>Progetto Trieste 2011, 4th round, Veterinary Drug Residues Proficiency Testing Service by Test Veritas S.r.l. </p><p>TEST MATERIAL: MI1133A-1 and MI1133A-2 (confirmatory) TETRACYCLINE and QUINOLONES IN LYOPHILIZED MILK - spiked 2011, 4th round</p><p>Test material A are two different samples: A-1 and A-2 - please test both materials!</p><p>LABORATORY: … ANALYST: ... DATE: ...</p><p>COMPOUNDS RESULTS SPECIFICATIONS DECISION CONCENTRATION DETECTION LIMIT ISO CORRECTED FOR RECOVERY CAPABILITY CC or 17025** MI1133A-1 RECOVERY* % CC cut-off yes/no (g/kg) (g/kg) (g/kg) OXYTETRACYCLINE EPIOXYTETRACYCLINE CHLORTETRACYCLINE EPICHLORTETRACYCLINE DOXYCYCLINE EPIDOXYCYCLINE TETRACYCLINE EPITETRACYCLINE ENROFLOXACIN CIPROFLOXACIN FLUMEQUINE MARBOFLOXACIN DANOFLOXACIN SARAFLOXACIN NALIDIXIC ACID OXOLINIC ACID Milk density = 1.03</p><p>Please indicate the concentration in relation to liquid milk sample (not of the powder)</p><p>A Maximum Residue Limits (MRL) of 100 g/kg for tetracycline, chlortetracycline and oxitetracyclin in milk has been definited by the European Commission (EU Regulation 37/2010). Doxycyclin is not allowed in dairy cows. A Maximum Residue Limit (MRL) in milk has been definited by the European Commission (EU Decision 37/2010) for some quinolones, as follows: 100 g/kg for enrofloxacin and ciprofloxacin (sum); 30 g/kg for danofloxacin; 50g/kg for flumequine; 75 g/kg for marbofloxacin. Oxolinic acid is not allowed in dairy cows.</p><p>TEST MATERIAL: MI1133A-1 and MI1133A-2 (confirmatory) TETRACYCLINE and QUINOLONES IN LYOPHILIZED MILK - spiked PAGINA 1 di 5 REVISIONE DATA DELLA REVISIONE DOCUMENTO AGGIORNATO IL 17/10/11 N. 0 03/01/2011 The data of your analyses will be kept for 5 years and after then will be destroyed. Progetto Trieste 2011, 4th round, Veterinary Drug Residues Proficiency Testing Service by Test Veritas S.r.l. </p><p>2011, 4th round</p><p>COMPOUNDS RESULTS SPECIFICATIONS DECISION CONCENTRATION DETECTION LIMIT ISO CORRECTED FOR RECOVERY CAPABILITY CC or 17025** MI1133A-2 RECOVERY* % CC cut-off yes/no (g/kg) (g/kg) (g/kg) OXYTETRACYCLINE EPIOXYTETRACYCLINE CHLORTETRACYCLINE EPICHLORTETRACYCLINE DOXYCYCLINE EPIDOXYCYCLINE TETRACYCLINE EPITETRACYCLINE ENROFLOXACIN CIPROFLOXACIN FLUMEQUINE MARBOFLOXACIN DANOFLOXACIN SARAFLOXACIN NALIDIXIC ACID OXOLINIC ACID Milk density = 1.03</p><p>Please indicate the concentration in relation to liquid milk sample (not of the powder)</p><p>Comments:</p><p>* Please indicate:  estimated concentration corrected with recovery if the compound is detected;  "< of…" if the compound is not detected;  "NS" if the compound is not searched (see example above reported).</p><p>**Please indicate whether the method used is in the scope of accreditation (choose “yes” if the methods is already accreditated).</p><p>TEST MATERIAL: MI1133A-1 and MI1133A-2 (confirmatory) TETRACYCLINE and QUINOLONES IN LYOPHILIZED MILK - spiked 2011, 4th round</p><p>PAGINA 2 di 5 REVISIONE DATA DELLA REVISIONE DOCUMENTO AGGIORNATO IL 17/10/11 N. 0 03/01/2011 The data of your analyses will be kept for 5 years and after then will be destroyed. Progetto Trieste 2011, 4th round, Veterinary Drug Residues Proficiency Testing Service by Test Veritas S.r.l. </p><p>Example: COMPOUNDS RESULTS SPECIFICATIONS CONCENTRATIO DECISION DETECTION N ISO RECOVER LIMIT CAPABILITY CORRECTED 17025** Y % CC CC FOR RECOVERY* yes/no (g/kg) (g/kg) (g/kg) Compound 1 150 90 80 95 y Compound 2 NS - - - - Compound 3 < 50 - 50 70 n</p><p>LABORATORY: … ANALYST: …</p><p>MARK YOUR CHOICE </p><p>Analytical methods used by participants Methods HPLC/MS UPLC/MS/MS HPLC/MS/MS GC/MS HPLC/DAD Other (specify)</p><p>Is the analytical method a routine one? Yes No</p><p>Source of standards for chromatographyc analysis OTC CTC DTC TC EPIMERS Sigma, Aldrich, Fluka Riedel-de Haen Dr. Ehrenstorfer Other (specify)</p><p>ENRO CIPRO FLUM MARB DAN SARA NAL. AC OXO.AC Sigma, Aldrich, Fluka Riedel-de Haen Dr. Ehrenstorfer Other (specify)</p><p>Sample preparation Amount of test sample for the extraction Sample volume (ml) 1 5 2 10 3 Other (specify)</p><p>Sample treatment Extraction dichloromethane Mc Ilvaine buffer ethyl acetate succinate buffer acetonitrile chloroform / acetone dichloromethane / trichloroacetic Other (specify) Digestion … (specify)</p><p>TEST MATERIAL: MI1133A-1 and MI1133A-2 (confirmatory) TETRACYCLINE and QUINOLONES IN LYOPHILIZED MILK - spiked 2011, 4th round</p><p>LABORATORY: … ANALYST: …</p><p>PAGINA 3 di 5 REVISIONE DATA DELLA REVISIONE DOCUMENTO AGGIORNATO IL 17/10/11 N. 0 03/01/2011 The data of your analyses will be kept for 5 years and after then will be destroyed. Progetto Trieste 2011, 4th round, Veterinary Drug Residues Proficiency Testing Service by Test Veritas S.r.l. </p><p>Clean up (SPE or other) SPE clean up C18 OASIS® Silica StrataTM SCX Other (specify) Other clean up n-hexane centrifugation filtration Other (specify)</p><p>HPLC methodology and conditions HPLC Gradient Isocratic Column phase C8 PFP C18 Other (specify) Column length (cm) 5 20 10 25 15 Other (specify) Column diameter (mm) 2 3.9 2.1 4.6 3 Other (specify) Particle size (m) 1.7 4 2.5 5 3 Other (specify) Cromatographyc column (type) AtlantisTM Prodigy® AcquityTM Symmetry® Beckman Synergi® GeminiTM Superspher® Hypersil® SupelcosilTM Hypercab® Ultrabase® HyPURITY X-terra® Lichrospher® YMCTM Luna® Zebron® Novapak® Zorbax® Nucleodur® Other (specify) Mobil phase acetonitrile / acetate buffer sodium acetate buffer / acetonitrile ammonium acetate / acetonitrile formic acid / acetonitrile water / acetonitrile / acetic acid formic acid / oxalic acid / acetonitrile acetate buffer Other (specify) pH of mobile phase x < 2 4 < x < 5 2 < x < 3 5 < x < 6 3 < x < 4 Other (specify) Flow rate (ml/min) 0.25 0.7 0.3 1 0.4 Other (specify) Post column reagent … (specify) TEST MATERIAL: MI1133A-1 and MI1133A-2 (confirmatory) TETRACYCLINE and QUINOLONES IN LYOPHILIZED MILK - spiked 2011, 4th round</p><p>LABORATORY: … ANALYST: …</p><p>Injection volume (l) 10 50 PAGINA20 4 di 5 REVISIONE DATA DELLA REVISIONE 100 DOCUMENTO AGGIORNATO IL 17/10/11 N. 0 03/01/2011 30 Other (specify) The data of your analyses will be kept for 5 years and after then will be destroyed. UV(nm) … (specify) Progetto Trieste 2011, 4th round, Veterinary Drug Residues Proficiency Testing Service by Test Veritas S.r.l. </p><p>GC methodology GC Capillary column length (m) … (specify) Film thickness (m) … (specify) Cromatographyc column Agilent Zorbax WCOT Other (specify) Zebron® Injection volume (l) … (specify) Injection temperature (°C) … (specify) Injection procedure Splitless Other (specify) Oven temperature (°C) … (specify)</p><p>Number of replicates (1 replicates = 1 extracion) Number of extraction 1 Other (specify) 2</p><p>Recovery (HPLC and GC) Recovery calculated by Internal standard Matrix matched calibration Spiked sample Other (specify) In-house Reference Material (RM)</p><p>Quality (HPLC and GC) Quality control implemented Control chart with in-house Duplicate analyses Reference Material (RM) Control chart with Certified Spiked sample Reference Material (CRM) Regular partecipation to Other (specify) proficency test (PT)</p><p>Reference (HPLC and GC) Reference Internal method Other (specify)</p><p>PAGINA 5 di 5 REVISIONE DATA DELLA REVISIONE DOCUMENTO AGGIORNATO IL 17/10/11 N. 0 03/01/2011 The data of your analyses will be kept for 5 years and after then will be destroyed.</p>