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Development of a capillary gas chromatographic method with flame ionisation detection for the simultaneous determination of sildenafil and its N ‐demethylated metabolite in biological fluids
Author(s) -
Berzas Nevado J. J.,
Villaseñor Llerena M. J.,
Contento Salcedo A. M.,
Rodríguez Flores Juana
Publication year - 2002
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 - 10.1002/1615-9314(20020801)25:12<767::aid-jssc767>3.0.co;2-0
Subject(s) - chromatography , chemistry , metabolite , flame ionization detector , gas chromatography , mass spectrometry , solid phase extraction , detection limit , urine , quantitative analysis (chemistry) , extraction (chemistry) , biochemistry
A simple, rapid, and sensitive method has been developed for the analysis of sildenafil (S) and its N ‐Demethylated metabolite UK‐103,320 (UK) using capillary gas chromatography with a flame ionisation detector. Optimal conditions were investigated, achieving analysis times shorter than 12 minutes. Aspects such as stability of the solutions, linearity, accuracy (<91%), precision, specificity, and limits of detection (0.02 mg/L and 0.12 mg/L for S and UK respectively) were tested in order to validate the method. A solid‐phase extraction (SPE) prior to the analysis allows quantification of S in serum and urine, and UK in serum at clinically relevant concentrations. Furthermore the specificity has been assessed by means of mass spectrometry in SCAN mode.