期刊
JOURNAL OF CHROMATOGRAPHY B
卷 748, 期 2, 页码 369-381出版社
ELSEVIER SCIENCE BV
DOI: 10.1016/S0378-4347(00)00355-8
关键词
oxytetracycline; tetracycline; chlortetracycline; mass spectrometry; LC-MS; frit FAB; particle beam
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(R) LRC cartridge. A 3 mum Spherisorb(R) 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. (C) 2000 Elsevier Science BN. All rights reserved.
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