Preliminary assays to elucidate the structure of oxytetracycline's degradation products in sediments. Determination of natural tetracyclines by high-performance liquid chromatography-fast atom bombardment mass spectrometry.
A very specific high-performance liquid chromatography-mass spectrometric method for the determination of natural tetracyclines was developed in order to characterise the degradation products of oxytetracycline in sediments. First, extraction used a clean up step with a Bond Elut Certify LRC cartridge. A 3 microm Spherisorb ODS1 column was then used with a methanol, acetonitrile and oxalic acid mobile phase gradient. Chromatographic resolution in these conditions was 3.31 between oxytetracycline and tetracycline. Two liquid chromatography-mass spectrometry methodologies based on a particle beam and a frit fast atom bombardment interface were developed. In the first approach, ionisation was performed in the negative chemical mode using methane as reacting gas. In the other case, glycerol-thioglycerol mixture was used as matrix to ensure good sensitivity. MS-MS experiment was performed to determinate oxytetracycline fragmentation pattern in the perspective of degradation product study.
Delépée
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R
Unité mixte de recherche INRA/ENVN, Chimiothérapie Aquacole et Environnement, Ecole Nationale Véterinaire de Nantes, Atlanpôle-La Chantrerie, France. rdelepee@vet-nantes.fr
Maume
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D
Le Bizec
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Pouliquen
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H
D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D015394:Molecular Structure; D010118:Oxytetracycline / Q000032:analysis / Q000737:chemistry*; D012680:Sensitivity and Specificity; D016339:Spectrometry, Mass, Fast Atom Bombardment; D014874:Water Pollutants, Chemical / Q000032:analysis*
D014874:Water Pollutants, Chemical; D010118:Oxytetracycline