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Determination of the stereoisomers in aqueous medium and serum and validation studies of racemic aminoalkanol derivatives of 1,7‐dimethyl‐8,9‐diphenyl‐4‐azatricyclo[5.2.1.0 2,6 ]dec‐8‐ene‐3,5,10‐trione, potential new anticancer drugs, by capillary electrophoresis
Author(s) -
Grodner Błażej,
Łukaszkiewicz Jacek,
Napiórkowska Mariola
Publication year - 2016
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.201600182
Subject(s) - chemistry , detection limit , chromatography , repeatability , enantiomer , aqueous solution , analyte , extraction (chemistry) , matrix (chemical analysis) , analytical chemistry (journal) , stereochemistry , organic chemistry
A new method for the determination of the stereoisomers, in aqueous medium and serum, of the racemic aminoalkanol derivatives I and II of 1,7‐dimethyl‐8,9‐diphenyl‐4‐azatricyclo[5.2.1.0 2,6 ]dec‐8‐ene‐3,5,10‐trione, which were found in earlier studies to be potential anticancer drugs, was developed and validated. The optimized conditions included 25 mM phosphate buffer adjusted to pH 2.5, containing γ‐cyclodextrin at a concentration of 5% m/v, as background electrolyte, an applied voltage of +10 kV, and a temperature of 25°C. Separations were carried out using a fused‐silica capillary. The developed method of determining the enantiomers of compounds I( S ), I( R ) and II( S ), II( R ) was characterized by the following parameters: a detection time within 10.8 min, a detection limit in the range of 141.2–141.7 ng/mL using the UV absorption detection at 200 nm. Good linearity ( R 2 = 0.9989–0.9998) was achieved within the range of concentrations studied. A very good extraction yield of 95.4–99.7% was achieved, and recoveries were carried out from both aqueous solutions and matrix serum. The repeatability of the method for peak areas with an accuracy of the determined concentrations of the analytes in the range of 1.43–1.89%, and limits of quantitation in the range of 432.4–436.3 ng/mL were achieved.