Analysis of felodipine by packed column supercritical fluid chromatography with electron capture and ultraviolet absorbance detection.
A reproducible and selective supercritical fluid chromatography (SFC) method was developed for the analysis of felodipine, a drug indicated for the treatment of hypertension. Methanol-modified carbon dioxide was employed as the SFC mobile phase with both electron capture detection (ECD) and multi-wavelength detection (MWD) being used simultaneously for analyte determination. Chromatography limit of detection (LOD) and limit of quantitation (LOQ), linear dynamic range (LDR) and injection precision were obtained in order to assess chromatographic and detector performance for both the SFC/MWD and SFC/ECD/MWD systems. The method was shown to be stability indicating since felodipine could be separated from its potential oxidative degradation product, H152/37, in under 6 min (felodipine k' = 2.44). Sample throughput was increased by 60% with the SFC assay vs LC. The optimized SFC method was shown to be equivalent to an existing LC/UV procedure for the analysis of a sustained-release tablet while realizing a 92% saving in disposable solvent waste. In order to achieve further solvent savings overall, supercritical fluid extraction (SFE) with 8% methanol-modified carbon dioxide as the extraction fluid was used to extract felodipine from a sustained-release tablet (as opposed to traditional solvent extraction). Comparable drug recoveries were obtained with SFE sample preparation technique when either SFC or LC extract analysis was utilized.
Strode
J T
JT
Department of Chemistry, Virginia Polytechnic Institute, Blacksburg, VA 24061.
Taylor
L T
LT
Howard
A L
AL
Ip
D
D
Brooks
M A
MA
D002853:Chromatography, Liquid / Q000379:methods*; D003692:Delayed-Action Preparations; D004563:Electrochemistry; D015736:Felodipine / Q000032:analysis*; D010084:Oxidation-Reduction; D012997:Solvents; D013056:Spectrophotometry, Ultraviolet
D003692:Delayed-Action Preparations; D012997:Solvents; D015736:Felodipine