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    Residues of ß-lactam antibiotics in bovine milk: confirmatory analysis by liquid chromatography tandem mass spectrometry after microbial assay screening

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    A procedure for the simultaneous determination of the residues of seven -lactam antibiotics (penicillin G, ampicillin, oxacillin, amoxicillin, dicloxacillin, cephalexin, cephapirin) in bovine raw milk using tandem liquid chromatography mass spectrometry (LC-MS/ MS) is described. The antibiotics were extracted by an acetic acid solution after centrifugation and filtration. The -lactams were separated using reversed-phase liquid chromatography. A triple quadrupole mass spectrometer was used in positive-ion mode as a detector via a Turbo Ionspray interface for electrospray ionization (ESI). The limits of detection and quantitation of the method were below the legal tolerances, except for ampicillin. The method was used to confirm 53samples found positive by a microbial method (Delvotest SP) at the Istituto Zooprofilattico Sperimentale per la Lombardia e l’Emilia Romagna of Brescia during 2001. Penicillin G was found in 26 samples at concentrations ranging from less than 4 to 6240550g l1. Amoxicillin was found in three samples at concentrations ranging from 8.50.1 to 53.72.3g l1. Cephapirin was found in two samples at 5.70.1 and 6.40.3 g l1

    Prevalence of molecules of b-lactam antibiotics in bovine milk in Lombardia and Emilia Romagna (Italy)

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    Gli autori riportano i risultati di una indagine preliminare sui livelli di contaminazione di latte e carne prodotti con il sistema biologico o con i metodi tradizionali da parte di pesticidi organoclorurati, policlorobifenili, piombo, cadmio e micotossine. I residui di pesticidi e policlorobifenili sia nel latte che nella carne biologici o convenzionali sono inferiori a limiti di legge e solo poche molecole sono state osservate in un numero limitato di campioni. I residui di cadmio e piombo sono pure molto bassi e non presentano differenze tra prodotti biologici e tradizionali. Il contenuto di aflatossina M1 nel latte biologico è significativamente maggiore di quello riscontrato nel latte convenzionale. Un quarto circa dei campioni (29 di tipo biologico e 7 di tipo convenzionale) supera il limite di 50 ppt previsto per il latte vaccino dal Regolamento CE 466/2001. La contaminazione da aflatossina M1 nel latte sembra essere un problema di azienda

    Residues of b-lactam antibiotics in bovine milk: HPLC-MS/MS confirmatory analysis after microbial assay screening

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    The analysis to detect antimicrobial residues in milk are usually performed in two steps: first, a microbiological method, based on the inibition of microbial growth, is used as a screening tool. Second the samples found positive are confirmed by a chernical method. A confirmatory method has to be able to detect which molecule is present in the sample and to quantitate it. HPLC-UV is the technique usually adopted as a confirmatory method. The use of this technique has some limitations. We developed a very fast chernical method based on HPLC-MS/MS. This method is able to process a great number of samples per day, giving an error-proof confirmation and with a very high sensitivity. The method has been validated and tested on 27 bovine milk samples found positive by a microbioiogical method at the IZSLER of Brescia
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