Liquid Chromatographic and Potentiometric Methods for Determinations of Clopidogrel

以液相層析法及雷位测量法檢测Clopidogrel

Amr Lotfy Saber ； Mohmed Alaa Elmosallamy ； Alaa Alside Amin ； Hamada Mohmed Ahmed Killa

《藥物食品分析》 16卷2期 (2008/04) Pp. 11-18

摘要

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法之分析條件爲：Nova-Pak(上標 ®) C18管柱(3.9mm×150mm，5μm)、以甲酸調整至pH=4之甲酸胺緩衝溶液/乙腈(40:60, v/v)爲移動相、檢測波長爲225nm。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 離子對作爲電流驅動物質，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。平均回收率爲100.6%，平均標準偏差爲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。

關鍵字

HPLC ； 電位測定法 ； 藥物分析 ； clopidogrel檢測

並列摘要

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(superscript ®) 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.

並列關鍵字

HPLC ； potentiometry ； pharmaceutical analysis ； clopidogrel determination