高效薄層層析法分析 nadifloxacin 微型乳劑及原料藥劑   全文下載

Validated Stability-Indicating Thin Layer Chromatographic Determination of Nadifloxacin in Microemulsion and Bulk Drug Formulations

本研究利用高效薄層層析法分析微型乳劑中nadifloxacin成分，並依國際醫藥法規協和會（ICH）原則確效。於吸光值288 nm，chloroform : methanol : formic acid（7.5 : 2.0 : 0.5, v/v）為移動相之分析條件，nadifloxa-cin阻滯係數為0.39 ± 0.02。濃度範圍50-600 ng/spot內，線性迴歸系數 r2 = 0.9981。偵測極限及定量極限分別為9.35及20.49 ng。酸鹼水解、氧化、光降解及熱處理等都會使藥物產生變化，比較阻滯係數（Rf）值，可區分標準品與降解物。統計分析顯示，高效薄層層析法分析nadifloxacin製劑具有再現性、選擇性及準確性，可有效區分藥物及其降解物，並應用為穩定性試驗方法。"

A stability-indicating high performance thin layer chromatographic (HPTLC) method for the densitometric analysis of nadi-floxacin in microemulsions was developed and validated according to the guidelines of the International Conference on Harmoniza-tion (ICH). The compact spot for nadifloxacin was found at an Rf value of 0.39 ± 0.02 at an absorption wavelength of 288 nm using a mobile phase consisting of chloroform : methanol : formic acid (7.5 : 2.0 : 0.5 v/v). The linear regression data for the calibration plots (r2 = 0.9981) was found with respect to peak area in the concentration range of 50 - 600 ng/spot. The limit of detection (LOD) and limit of quantification (LOQ) were 9.4 and 20.5 ng respectively. The drug was subjected to acid and alkaline hydrolysis, oxidation, photo degradation and dry heat treatment. The peaks of degradation products were well-resolved from the peak of the standard drug with significantly different Rf values. Statistical analysis revealed that the developed HPTLC method is reproducible, selective and accurate for the determination of nadifloxacin in its formulations. The method can effectively separate the drug from its degradation products and be used for stability-indicating assay.