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An LC-MS method is described for the confirmation of six quinolones (enrofloxacine, ciprofloxacine, marbofloxacine, danofloxacine, sarafloxacine and difloxacine) in pig muscle. The quinolones were extracted from muscle (2 g) with phosphate buffer (pH 7.4). After centrifugation, the extract was purified on a C18 solid-phase extraction cartridge. Samples were analysed by LC with gradient elution on a C18 column and detected by MS via an atmospheric pressure chemical ionisation interface. For each compound, an intense pseudo-molecular ion [M+H]+ is obtained. The assay is specific and reproducible and allows the confirmation of the six quinolones at the 7.5 micrograms kg-1 level in pig muscle.

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A particle beam/liquid chromatographic/mass spectrometric (PB/LC/MS) method capable of determining 5 macrolides in bovine muscle is described. Spiramycin, tylosin, tilmicosin, erythromycin, and josamycin residues in bovine muscle are confirmed by reversed-phase LC/MS incorporating gradient elution. Macrolides are extracted from tissue with chloroform, and the extract is purified with a diol solid-phase extraction cleanup. The 5 macrolides are identified by negative and positive chemical ionization with selective ion monitoring of 2 ions in each mode. The procedure confirms the presence of each macrolide at 50 μg/kg in spiked samples.

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Spiramycin is a macrolide antibiotic that is active against most of the microorganisms isolated from the milk of mastitic cows. This work investigated the disposition of spiramycin in plasma and milk after intravenous, intramuscular and subcutaneous administration. Twelve healthy cows were given a single injection of spiramycin at a dose of 30,000 IU/kg by each route. Plasma and milk were collected post injection. Spiramycin concentration in the plasma was determined by a high performance liquid chromatography method, and in the milk by a microbiological method. The mean residence time after intravenous administration was significantly longer (P less than 0.01) in the milk (20.7 +/- 2.7 h) than in plasma (4.0 +/- 1.6 h). An average milk-to-plasma ratio of 36.5 +/- 15 was calculated from the area concentration-time curves. Several pharmacokinetic parameters were examined to determine the bioequivalence of the two extravascular routes. The dose fraction adsorbed after intramuscular or subcutaneous administration was almost 100% and was bioequivalent for the extravascular routes, but the rates of absorption, the maximal concentrations and the time to obtain them differed significantly between the two routes. Spiramycin quantities excreted in milk did not differ between the two extravascular routes but the latter were not bioequivalent for maximal concentration in the milk. However, the two routes were bio-equivalent for the duration of time the milk concentration exceeded the minimal inhibitory concentration (MIC) of various pathogens causing infections in the mammary gland.(ABSTRACT TRUNCATED AT 250 WORDS)

A particle beam liquid chromatography-mass spectrometric method is presented as a confirmatory technique for analysis of tylosin residues in bovine muscle. After chloroform extraction and a diol solid-phase extraction clean-up, on-line liquid chromatography-mass spectrometry (LC-MS) of extracts is carried out on an RP-18 bonded silica column. The analyte is introduced into the ion source by a particle beam interface and identified by negative chemical ionization with selective ion monitoring. The tylosin molecular ion is obtained with this ionization mode. The response of the ion chromatogram peak areas is linear for the three levels of spiked muscle analysed (0.5, 1 and 2 maximum residue limit). Under these LC-MS conditions, other macrolide antibiotics such as spiramycin and erythromycin do not interfere with tylosin.

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 micrograms 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 micrograms kg-1.