title: Determination of gliclazide in pharmaceutical preparations by capillary gas chromatography with cool on-column injection and elimination of the matrix effect.
abstract: Conditions were established for the identification and quantitation of gliclazide in pharmaceutical preparations by capillary gas chromatography with flame ionization detection and cool on-column injection. Gliclazide was extracted with methanol and, after filtration, assayed on a (25 m x 0.25 mm id, 0.2 microm film thickness) CP-WAX 58 (FFAP)-CB WCOT fused silica column. Because the available preparations were of various origins and, therefore, could differ in auxiliary substances and their qualitative parameters, the influence of the matrix constituents on the analytical results was taken into account. Good separation conditions were established for the developed method. The retention time of gliclazide is about 36 min and differs from the retention times of the internal standard (approximately 29 min) and additional peaks present in chromatograms (20-26 min), which were assigned to matrix constituents. The recoveries of gliclozide were high and reached 96.5%. The developed method is characterized by selectivity and precision (relative standard deviation 0.38-1.26%), a wide range of linearity (0.1-10.0 mg/mL), and a limit of detection of 30 ng. In addition, the results of chromatographic analyses calculated in 3 ways were compared with those obtained by UV spectrophotometry. The suggested technique of cool on-column injection, in contrast with split-splitless injection (used in preliminary investigations), reduces to a minimum the possibility of thermal decomposition of gliclazide.
authors.affiliation: Jagiellonian University, Collegium Medicum, Department of Inorganic and Analytical Chemistry, Kraków, Poland. mfczekaj@cyf-kr.edu.pl
authors.forename: J
authors.initials: J
authors.lastname: Krzek
authors.forename: J
authors.initials: J
authors.lastname: Czekaj
authors.forename: M
authors.initials: M
authors.lastname: Moniczewska
authors.forename: W
authors.initials: W
authors.lastname: Rzeszutko
mesh_terms: D002849:Chromatography, Gas / Q000379:methods* / Q000706:statistics & numerical data; D005410:Flame Ionization / Q000379:methods / Q000706:statistics & numerical data; D005907:Gliclazide / Q000008:administration & dosage / Q000032:analysis*; D006801:Humans; D007004:Hypoglycemic Agents / Q000008:administration & dosage / Q000032:analysis*; D004364:Pharmaceutical Preparations / Q000008:administration & dosage / Q000032:analysis*; D012680:Sensitivity and Specificity; D012996:Solutions; D013056:Spectrophotometry, Ultraviolet
chemical_list: D007004:Hypoglycemic Agents; D004364:Pharmaceutical Preparations; D012996:Solutions; D005907:Gliclazide