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Determination of new pyridoquinoline derivatives and their quantification in urine by capillary liquid chromatography
Author(s) -
Srbek Jan,
Coufal Pavel,
Tesařová Eva,
Bosáková Zuzana,
Suchánková Jana
Publication year - 2003
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.200301557
Subject(s) - chromatography , chemistry , calibration curve , triethylamine , detection limit , quantitative analysis (chemistry) , capillary action , matrix (chemical analysis) , analytical chemistry (journal) , impurity , phase (matter) , high performance liquid chromatography , methanol , materials science , organic chemistry , composite material
Capillary liquid chromatography (CLC) in reversed separation mode was applied to the quantification and impurity profile determination of eight newly synthesized pyridoquinolines. The CLC separation system consisted of Nucleosil C18 stationary phase and methanol containing 1% ( v/v ) of triethylamine (TEA) as the mobile phase. The optimized separation system enabled the separation of impurities from the main component and their quantification in a reasonable analysis time. The presence of TEA in the mobile phase greatly improved the peak shape and decreased the analysis time of the studied derivatives on the C18 stationary phase. Calibration curves of pyridoquinolines were plotted in a concentration range from 1.0×10 –6 to 1.0×10 –3 mol/L at two parallel detector wavelengths of 254 and 265 nm and subsequently used for quantification of pyridoquinoline derivatives in human urine. No pretreatment of the real biological sample was needed. Detection and quantification limits were calculated for all the derivatives and the detection limits of most of the pyridoquinolines were found to lie in the μmol/L concentration range. The proposed CLC separation system has proved to be a suitable method for quantification of test derivatives in samples containing human urine matrix.