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Development of a liquid chromatography/electrospray tandem mass spectrometry method for confirmation of chloramphenicol residues in milk after alfa‐1‐acid glycoprotein affinity chromatography
Author(s) -
Gallo Pasquale,
Nasi Antonella,
Vinci Floriana,
Guadagnuolo Grazia,
Brambilla Gianfranco,
Fiori Maurizio,
Serpe Luigi
Publication year - 2005
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/rcm.1825
Subject(s) - chemistry , chromatography , electrospray , liquid chromatography–mass spectrometry , tandem mass spectrometry , mass spectrometry , selected reaction monitoring , affinity chromatography , veterinary drug , repeatability , electrospray ionization , biochemistry , enzyme
In this work we present a method for confirmatory analysis of chloramphenicol (CAP) in bovine and buffalo raw milk. CAP is extracted in acetonitrile and purified by affinity chromatography on an α ‐1‐acid glycoprotein (AAG) column, then is identified and determined by ion‐trap liquid chromatography/electrospray ionisation tandem mass spectrometry (LC/ESI‐MS/MS) analysis in the negative ion mode. CAP was identified at the minimum required performance limit (MRPL) of 0.30 ppb, by monitoring the [M–H] − ion and at least two product ions, meeting the qualitative and quantitative criteria set by the European Commission in Decision 2002/657/EC for confirmation of prohibited veterinary drugs. The trueness and within‐day and between‐day repeatability data are also reported. Moreover, the loading capacity of affinity columns towards CAP was tested. This method, based on the molecular recognition between drug and AAG during the purification step to improve sample cleanup, represents a quantitative and repeatable procedure for confirmatory analysis, and fits the requirements for the routine official control of CAP residues in raw milk. Copyright © 2005 John Wiley & Sons, Ltd.