Multi-component analysis of tetracyclines, sulfonamides and tylosin in swine manure by liquid chromatography-tandem mass spectrometry

A multi-component method focussing on thorough sample preparation has been developed for simultaneous analysis of swine manure for three classes of antibiotic--tetracyclines, sulfonamides, and tylosin. Liquid manure was initially freeze-dried and homogenised by pulverization before extraction by pre...

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Bibliographic Details
Published in:Analytical and bioanalytical chemistry 2006-03, Vol.384 (5), p.1164-1174
Main Authors: Jacobsen, Anne Marie, Halling-Sørensen, Bent
Format: Article
Language:English
Subjects:
Animals
Antibiotics
Calibration
Chromatography, Liquid - methods
Citric acid
Dry matter
Formic acid
Heptanes
Hogs
LC-ESI-MS-MS
Lipids
Liquid chromatography
Liquid manure
Liquid-liquid extraction
Manure
Manure - analysis
Manures
Mass spectrometry
Mass spectroscopy
Oxytetracycline
pH effects
Pig manure
Pressure
Sample preparation
Sensitivity and Specificity
Signal to noise ratio
Sulfadiazine
Sulfonamides
Sulfonamides - analysis
Swine
Swine production
Tandem Mass Spectrometry - methods
Temperature
Tetracyclines
Tetracyclines - analysis
Time Factors
Tylosin
Tylosin - analysis
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Summary:A multi-component method focussing on thorough sample preparation has been developed for simultaneous analysis of swine manure for three classes of antibiotic--tetracyclines, sulfonamides, and tylosin. Liquid manure was initially freeze-dried and homogenised by pulverization before extraction by pressurised liquid extraction. The extraction was performed at 75°C and 2,500 psig in three steps using two cycles with 0.2 mol L-¹ citric acid buffer (pH 4.7) and one cycle with a mixture of 80% methanol with 0.2 mol L-¹ citric acid (pH 3). After liquid-liquid extraction with heptane to remove lipids, the pH of the manure was adjusted to 3 with formic acid and the sample was vacuum-filtered through 0.6 μm glass-fibre filters. Finally the samples were pre-concentrated by tandem SPE (SAX-HLB). Recoveries were determined for manure samples spiked at three concentrations (50-5,000 μg kg-¹ dry matter); quantification was achieved by matrix-matched calibration. Recoveries were >70% except for oxytetracycline (42-54%), sulfadiazine (59-73%), and tylosin (9-35%) and did not vary with concentration or from day-to-day. Limits of quantification (LOQ) for all compounds, determined as a signal-to-noise ratio of 10, were in the range 10-100 μg kg-¹ dry matter. The suitability of the method was assessed by analysis of swine manure samples from six different pig-production sites, e.g. finishing pigs, sows, or mixed production. Residues of antibiotics were detected in all samples. The largest amounts were found for tetracyclines (up to 30 mg kg-¹ dry matter for the sum of CTC and ECTC). Sulfonamides were detected at concentrations up to 2 mg kg-¹ dry matter (SDZ); tylosin was not detected in any samples. [graphic removed]
ISSN:1618-2642
1618-2650
DOI:10.1007/s00216-005-0261-9