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Multiresidue determination of penicillins in environmental waters and chicken muscle samples by means of capillary electrophoresis‐tandem mass spectrometry
Author(s) -
BailónPérez M. Isabel,
GarcíaCampaña Ana M.,
del Olmo Iruela Monsalud,
CrucesBlanco Carmen,
Gracia Laura Gámiz
Publication year - 2009
Publication title -
electrophoresis
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.666
H-Index - 158
eISSN - 1522-2683
pISSN - 0173-0835
DOI - 10.1002/elps.200800732
Subject(s) - capillary electrophoresis , chromatography , mass spectrometry , tandem mass spectrometry , chemistry , tandem , environmental chemistry , materials science , composite material
A new analytical method based on CZE coupled with tandem MS detection (CE‐MS/MS) has been developed for the simultaneous determination of nine penicillins of human and veterinary use (nafcillin, dicloxacillin, cloxacillin, oxacillin, ampicillin, penicillin G, amoxicillin, penicillin V and piperacillin), whose levels are regulated by the EU Council regulation No. 2377/90 in animal edible tissues. CE separation conditions, sheath liquid composition and electrospray parameters have been carefully optimized to reach high sensitivity and precision. Separation was carried out in a 96 cm total length fused‐silica capillary (50 μm id, 360 μm od) using 60 mM ammonium acetate at pH 6.0 as running buffer. Lomefloxacin was used as internal standard. MS/MS experiments were carried out using an IT as analyzer operating in multiple reaction monitoring mode to achieve the minimum number of identification points established by the 2002/657/EC European Decision. The use of an SPE procedure in two steps, combining Oasis hydrophilic–liphophilic balance and Alumina N cartridges provide a satisfactory preconcentration and clean up treatment for meat samples after extraction of the compounds with ACN. Only Oasis hydrophilic–liphophilic balance cartridges were necessary in water samples to obtain adequate recoveries. The method has been characterized for its use in meat and water samples, using matrix‐matched calibrations. For chicken muscle samples, LODs between 8 and 12 μg/kg have been obtained, in all cases lower than the maximum residue limits permitted. For water samples LODs from 0.18 to 0.26 μg/L could ensure its satisfactory application in aquatic samples.