Komsta Lukasz, Misztal Genowefa
Medical University, Department of Medicinal Chemistry, 6 Chodzki, 20-093 Lublin, Poland.
J AOAC Int. 2005 Sep-Oct;88(5):1517-24.
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.
已开发出采用密度测定法和视频扫描检测的新型薄层色谱（TLC）方法，用于定量测定非诺贝特胶囊中的非诺贝特以及吉非贝齐片中的吉非贝齐。分析在高效TLC二醇F254板上进行，使用正己烷 - 四氢呋喃（8 + 2，v/v）流动相，在水平DS室中采用三明治技术。活性物质用甲醇从片剂中提取。密度测定法在227 nm处进行，视频扫描定量在254 nm处进行。两种药物均在5 - 30 μg/斑点（20 μL不同浓度溶液）范围内构建校准曲线。校准数据针对3种回归模型进行测试，并选择最佳模型（视频扫描为二次模型，密度测定法为非线性y = ax(m) + b，所有情况下R2 > 0.997）。通过点样不同量的提取溶液（15 - 30 mg/斑点）测试方法的线性。在所有情况下，回收率函数均具有足够的线性，截距不显著且斜率非常接近1。通过对3个加标样品（理论值的50%、100%和150%）进行定量测试准确性，结果具有同质性且无显著差异。密度测定法中非诺贝特的回收率为101.42%（总相对标准偏差10.76%），吉非贝齐为100.47%（9.7%）。视频密度测定法的回收率分别为102.73%（12.59%）和98.79%（8.56%）。两种方法的精密度和准确性的F - Snedecor检验和双样本t检验均未显示出显著差异。
