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Confirmatory analysis for spiramycin residue in bovine muscle by liquid chromatography/particle beam mass spectrometry
Author(s) -
Sanders P.,
Delépine B.
Publication year - 1994
Publication title -
biological mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.475
H-Index - 121
eISSN - 1096-9888
pISSN - 1052-9306
DOI - 10.1002/bms.1200230612
Subject(s) - chromatography , chemistry , mass spectrometry , maximum residue limit , detection limit , veterinary drug , spiramycin , residue (chemistry) , orbitrap , tylosin , liquid chromatography–mass spectrometry , chemical ionization , solid phase extraction , analytical chemistry (journal) , pesticide residue , ion , ionization , biochemistry , erythromycin , organic chemistry , pesticide , agronomy , biology , antibiotics
To ensure that residues of veterinary drugs, above their respective maximum residue limits, do not reach the human food supply, European Community regulations specify requirements for detection, quantification and confirmation analytical methods and control procedures. The European Community member states base meat controls on these protocols. A liquid chromatographic/mass spectrometric analysis of spiramycin in calf muscle is presented as a confirmatory method for this compound. A particle beam interface was used, with negative ion chemical ionization mass spectrometry, using methane as the reagent gas. Samples (2 g muscle were prepared by liquid/liquid extraction followed by solid‐phase extraction clean‐up. On‐line liquid chromatography/mass spectrometry of extracts was carried out on a C‐18 bonded silica column. The specificity required for a regulatory confirmation procedure was achieved by monitoring five fragment ions with m/z 304, 330, 475, 683 and 684. Variation of the relative ion abundances was less than 20% at the maximum limit of residue, 50 μg kg −1 . The method specificity was tested for three related compounds: neospiramycin, erythromycin and tylosin. The detection limit based on ion chromatogram peaks areas obtained with control samples was determined to be 20 μg kg −1 .