High-performance thin-layer chromatography with densitometry for the determination of ciprofloxacin and impurities in drugs.
A thin-layer chromatographic (TLC)-densitometric method has been developed for identification and quantification of ciprofloxacin (Rf = 0.61) and an ethylenediamine compound (Rf = 0.42), a desfluoro compound (Rf = 0.48), by-compound A (Rf = 0.53), and fluoroquinolonic acid (Rf = 0.68) as ciprofloxacin degradation products in pharmaceutical preparations. By using chloroform-methanol-25% ammonia (43 + 43 + 14, v/v/v) as the mobile phase and silica gel 60 F254 high-performance TLC plates as the stationary phase, it was possible to separate individual constituents that, when subjected to ultraviolet (UV) densitometric analysis at 330 nm for fluoroquinolonic acid and 277 nm for the other compounds, gave well developed peaks allowing easy qualitative and quantitative analyses. DMSO-methanol (1 + 1) was used to extract drug constituents. The method showed high sensitivity (limit of detection 10 to 44 ng), a wide linearity range (3 to 20 microg/mL), and good precision (2.32 to 6.46% relative standard deviation) and accuracy (percentage recoveries 98.62 to 101.52%) for individual constituents.
Krzek
Jan
J
Jagiellonian University, Collegium Medicum, Department of Inorganic and Analytical Chemistry, Medyczna 9, 30-688 Krakow, Poland. jankrzek@cm-uj.krakow.pl
Hubicka
Urszula
U
Szczepańiczyk
Justyna
J
D002855:Chromatography, Thin Layer / Q000379:methods*; D002939:Ciprofloxacin / Q000032:analysis*; D003720:Densitometry / Q000379:methods*; D004340:Drug Contamination; D004364:Pharmaceutical Preparations / Q000032:analysis* / Q000737:chemistry*; D012015:Reference Standards; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity
D004364:Pharmaceutical Preparations; D002939:Ciprofloxacin