Determination of fenofibrate and gemfibrozil in pharmaceuticals by densitometric and videodensitometric thin-layer chromatography.
New thin-layer chromatography (TLC) methods with densitometric and videoscanning detection were elaborated for the quantitative determination of fenofibrate in Fenoratio capsules and gemfibrozil in Gemfibral tablets. Analysis was performed on high-performance TLC diol F254 plates using hexane-tetrahydrofuran (8 + 2, v/v) mobile phase in horizontal DS chambers using the sandwich technique. The active substances were extracted from tablets with methanol. Densitometric assay was performed at 227 nm and videoscanning quantitation at 254 nm. Calibration plots were constructed in range 5-30 microg/spot (20 microL of solutions in different concentrations) for both of the drugs. The calibration data were tested against 3 regression models, and the optimum model was selected (quadratic for videoscanning and nonlinear y = ax(m) + b for the densitometric method, R2 > 0.997 in all cases). Linearity of the methods was tested by spotting different amounts of extracted solution (15-30 mg/spot). The recovery function was sufficiently linear in all cases, with an insignificant intercept and a slope very close to 1. Accuracy was tested by quantitating 3 fortified samples (50,100, and 150% of theoretical), and the results were homogeneous with no significant differences. The recovery in the densitometric assay was 101.42% (total relative standard deviation 10.76%) for fenofibrate and 100.47% (9.7%) for gemfibrozil. Videodensitometry resulted in recoveries of 102.73% (12.59%) and 98.79% (8.56%), respectively. The F-Snedecor test and Student's t-test for 2 means showed no significant differences between the precision and accuracy of both methods.
Komsta
Lukasz
L
Medical University, Department of Medicinal Chemistry, 6 Chodzki, 20-093 Lublin, Poland. kzchl@asklepios.am.lublin.pl
Misztal
Genowefa
G
D002138:Calibration; D002855:Chromatography, Thin Layer / Q000379:methods*; D003720:Densitometry / Q000379:methods*; D011345:Fenofibrate / Q000032:analysis*; D015248:Gemfibrozil / Q000032:analysis*; D004364:Pharmaceutical Preparations / Q000032:analysis* / Q000737:chemistry*; D012015:Reference Standards; D012044:Regression Analysis; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity
D004364:Pharmaceutical Preparations; D015248:Gemfibrozil; D011345:Fenofibrate