以液相層析法及電位測量法檢測Clopidogrel   全文下載

Liquid Chromatographic and Potentiometric Methods for Determinations of Clopidogrel

本研究中，兩種不同的技術被開發，並用於藥品製備中clopidogrel 之檢測。HPLC 法之分析條件為：Nova-PakR C18 管柱（3.9 mm × 150 mm，5 μm）、以甲酸調整至pH = 4 之甲酸胺緩衝溶液/ 乙?（40:60，v/v）為移動相、檢測波長為225 nm。結果呈現良好的線性（r = 0.9993）、準確度（ ? 99.20%）， 以及精確度（ ? 0.6 RSD）。電位測量是根據tetrakis （p-chlorophenyl） borate-clopidogrel 離子對作為電流驅動物質，將塑化的PVC膜與o-nitrophenyl octyl ether 或dioctyl phthalate 混合。使用前，感應器需於0.1 M 藥品溶液中調整至少2 天。結果顯示，clopidogrel 在濃度範圍1.0 × 10-5 ~ 1.0 × 10-2 M，pH 範圍1.5 ~ 4.0 時，呈現快速又穩定之Nernstian 反應。平均回收率為100.6%，平均標準偏差為0.86%。在許多陰離子的存在下，感應器對於clopidogrel hydrogen sulphate 顯示出不錯的選擇性。賦型劑和稀釋劑之間無顯著差異。

Two different techniques are developed for the determination of clopidogrel in pharmaceutical preparations. HPLC method has been developed where chromatographic analysis is performed on Nova-Pak® C18 column (3.9 mm × 150 mm, 5 μm) with an ammonium formate buffer adjusted with formic acid to pH 4.0, acetonitrile (40:60, v/v) as mobile phase, and detection at 225 nm. Good linearity (0.9993, r), accuracy (≥ 99.20 %), and precision (≤ 0.6 RSD) were obtained. Potentiometric measurments are based on tetrakis (p-chlorophenyl) borate-clopidogrel ion-pair as an electroactive material incorporating a plasticized PVC membrane with o-nitrophenyl octyl ether or dioctyl phthalate. The sensor is conditioned for at least two days in 0.1 M drug solution before use. It exhibits fast and stable Nernstian response for clopidogrel over the concentration range of 1.0 × 10-5 ~ 1.0 × 10-2 M and pH range of 1.5 - 4.0. Results with an average recovery of 100.6% and a mean standard deviation of 0.86% of the nominal were obtained. The sensor shows reasonable selectivity towards clopidogrel hydrogen sulphate in presence of many cations. No significant interferences are caused by drug excipients and diluents.