Analysis of Tetracycline, Oxytetracycline and Chlortetracycline in Plasma Extracts by Electrospray Tandem Mass-Spectrometry and by Liquid Chromatography

Weimann, Allan; Bojesen, Gustav; Nielsen, P. G.

doi:10.1080/00032719808005284

Cited by 17 publications

(7 citation statements)

References 9 publications

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“…It is clear that even when using such a selective detection technique as mass spectrometry (MS), the liquid chromatographic (LC) part of the method will have to ensure a complete separation of both components, in order to be able to quantify correctly mixtures of them present in tissue samples. Several LC-MS methods were described earlier to determine OTC residues in complex tissue matrices, [4][5][6][7][8] as well as in other matrices such as honey, 9 milk, 10 plasma 11 and ground and surface water. 12 However, none of these methods is able to quantify OTC and its 4-epimer separately.…”

Section: Introductionmentioning

confidence: 99%

Quantitative analysis of oxytetracycline and its 4-epimer in calf tissues by high-performance liquid chromatography combined with positive electrospray ionization mass spectrometry

Cherlet

Baere

Backer

2003

Analyst

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Tetracycline antibiotics are commonly used in veterinary medicine because of their broad spectrum activity and cost effectiveness. Oxytetracycline (OTC) is one of the most important members of this antibiotic family. The purpose of this study was to develop and validate a method to determine OTC residues in edible tissues of calf. Extraction of OTC and its 4-epimer (4-epiOTC), in the presence of the internal standard demethylchlortetracycline (DMCTC), was performed using a liquid extraction with sodium succinate solution (pH 4.0), followed by protein removal with trichloroacetic acid and paper filtration. Further solid-phase extraction clean-up on an HLB polymeric reversed phase column was performed to obtain an extract suitable for LC-MS-MS analysis. Chromatographic separation of the internal standard, and especially OTC and its 4-epimer, was achieved on a PLRP-S polymeric reversed phase column, using a mixture of 0.001 M of oxalic acid, 0.5% (v/v) of formic acid and 3% (v/v) of tetrahydrofuran in water (mobile phase A) and tetrahydrofuran (mobile phase B) as the mobile phase, and at a column temperature of 60 degrees C. OTC and its 4-epimer could be identified using the MS-MS detection technique, and were subsequently quantified. The method has been validated according to the requirements of the EC at the MRL (maximum residue limit, 100 ng g(-1) for muscle, 300 ng g(-1) for liver and600 ng g(-1) for kidney), half the MRL and double the MRL levels, as well for OTC as for 4-epiOTC. Calibration graphs were prepared for all tissues and good linearity was achieved over the concentration ranges tested (r > 0.99 and goodness of fit < 10%). Limits of quantification of half the MRLs were obtained for the analysis of OTC and 4-epiOTC in muscle, liver and kidney tissues of calf. Limits of detection ranged for both components between 0.8 and 48.2 ng g(-1). The within-day and between-day precisions, expressed as RSD values, were all below the maximum allowed RSD values calculated according to the Horwitz equation. The results for accuracy fell within the -20% to +10% range. Recoveries were between 47 and 56% for OTC, and between 52 and 62% for 4-epiOTC, depending on the tissue. The method has been successfully used for the quantitative determination of OTC and 4-epiOTC in tissue samples of calves medicated with OTC by intramuscular injection.

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Section: Introductionmentioning

confidence: 99%

Quantitative analysis of oxytetracycline and its 4-epimer in calf tissues by high-performance liquid chromatography combined with positive electrospray ionization mass spectrometry

Cherlet

Baere

Backer

2003

Analyst

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“…That method involves stacking an anion-exchange and an alumina SPE cartridge for the isolation of SAs. SPE methods also have been developed for SAs and TCs in blood, meat, and other biological matrixes. − Smallridge et al were among the first to extract sulfamethazine and sulfathiazole from swine feed. Online chromatographic separation 19,20 and liquid−liquid extraction 20 also have been used to separate SAs from a complex matrix.…”

mentioning

confidence: 99%

Analysis of Trace Levels of Sulfonamide and Tetracycline Antimicrobials in Groundwater and Surface Water Using Solid-Phase Extraction and Liquid Chromatography/Mass Spectrometry

2001

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A method has been developed for the trace analysis of two classes of antimicrobials consisting of six sulfonamides (SAs) and five tetracyclines (TCs), which commonly are used for veterinary purposes and agricultural feed additives and are suspected to leach into ground and surface water. The method used solid-phase extraction and liquid chromatography/mass spectrometry (LC/MS) with positive ion electrospray. The unique combination of a metal chelation agent (Na2EDTA) with a macroporous copolymer resulted in quantitative recoveries by solid-phase extraction (mean recovery, 98 +/- 12%) at submicrogramper-liter concentrations. An ammonium formate/formic acid buffer with a methanol/water gradient was used to separate the antimicrobials and to optimize the signal intensity. Mass spectral fragmentation and ionization characteristics were determined for each class of compounds for unequivocal identification. For all SAs, a characteristic m/z 156 ion representing the sulfanilyl fragment was identified. TCs exhibited neutral losses of 17 amu resulting from the loss of ammonia and 35 amu from the subsequent loss of water. Unusual matrix effects were seen only for TCs in this first survey of groundwater and surface water samples from sites around the United States, requiring that TCs be quantitated using the method of standard additions.

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“…Several methods have been reported for the determination of chlortetracycline hydrochloride, including spectrophotometry [1,2], high performance liquid chromatography [3,4], fluorimetry [5], room temperature phosphorescence [6], flow injection potentiometry [7], capillary electrophoresis [8], flow-injection chemiluminescence [9], and differential pulse polarography [10]. Electrodes selective for chlortetracycline of the conventional membrane type based on CTC-tungstosilicate ion-pair has been reported [11], however, the effective pH of the electrode was 5 and the detection limit was 30-40 mmol dm À3 .…”

Section: Introductionmentioning

confidence: 99%

Plastic Membrane Selective Electrodes for Chlortetracyclinium Ion Based on Chlortetracyclinium-Phosphotungstate and Phosphomolybdate Ion-Pair Associates

2001

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Analysis of Tetracycline, Oxytetracycline and Chlortetracycline in Plasma Extracts by Electrospray Tandem Mass-Spectrometry and by Liquid Chromatography

Cited by 17 publications

References 9 publications

Quantitative analysis of oxytetracycline and its 4-epimer in calf tissues by high-performance liquid chromatography combined with positive electrospray ionization mass spectrometry

Quantitative analysis of oxytetracycline and its 4-epimer in calf tissues by high-performance liquid chromatography combined with positive electrospray ionization mass spectrometry

Analysis of Trace Levels of Sulfonamide and Tetracycline Antimicrobials in Groundwater and Surface Water Using Solid-Phase Extraction and Liquid Chromatography/Mass Spectrometry

Plastic Membrane Selective Electrodes for Chlortetracyclinium Ion Based on Chlortetracyclinium-Phosphotungstate and Phosphomolybdate Ion-Pair Associates

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