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Determination of the Dihydropyridine Aryloxypropanolamine Z6568 and its Acidic Metabolites in Plasma, Urine and Tissues by Solid Phase Extraction and Liquid Chromatography/Negative‐ion Mass Spectrometry
Author(s) -
Gregori Mario,
Castelnovo Pierfrancesco
Publication year - 1996
Publication title -
journal of mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.475
H-Index - 121
eISSN - 1096-9888
pISSN - 1076-5174
DOI - 10.1002/(sici)1096-9888(199609)31:9<994::aid-jms365>3.0.co;2-g
Subject(s) - chemistry , chromatography , thermospray , mass spectrometry , solid phase extraction , extraction (chemistry) , detection limit , urine , liquid chromatography–mass spectrometry , chemical ionization , high performance liquid chromatography , selected reaction monitoring , tandem mass spectrometry , ion , ionization , biochemistry , organic chemistry
A sensitive and selective liquid chromatographic/mass spectrometric assay for the determination of the dihydropyridine aryloxypropanolamine compound Z6568 and its monoacidic metabolites in plasma, urine and tissues has been developed and validated. Z6568 and the acidic metabolites were isolated from the biological matrices by solid‐phase extraction, separated by reversed‐phase high‐performance liquid chromatography and detected by mass spectrometry using a thermospray interface. Filament ionization and negative‐ion detection were used, monitoring the molecular ion of Z6568 and a major fragment of the acidic metabolites. The analysis of spiked plasma, urine and tissues demonstrated good accuracy and precision of the assay with a detection limit of 0.5 ng ml ‐1 for Z6568 and 2 ng ml ‐1 for the metabolites. Data relative to the optimization of the extraction procedure, mass spectrometric conditions and the validation protocol are reported. The method was used to investigate the metabolic fate and tissue distribution in laboratory animals.