El-Bagary Ramzia I, Mohammed Nashwah G, Nasr Heba A
Pharmaceutical Chemistry Department, Faculty of Pharmacy, Cairo University, Cairo, Egypt.
Anal Chem Insights. 2012;7:13-21. doi: 10.4137/ACI.S8864. Epub 2012 May 14.
Two stability indicating chromatographic methods were proposed for the determination of almotriptan, eletriptan, and rizatriptan, in presence of their acid degradation products. The first method is a quantitative densitometric thin layer chromatography. The developing systems were; acetonitrile: methanol: dichloromethane: ammonia (10:6:3:1 v/v), ethyl acetate: methanol: ammonia (15:4:1 v/v), and methanol: acetonitrile: ammonia (9:4:1 v/v) for almotriptan, eletriptan and rizatriptan respectively. The TLC plates were scanned at 235 nm. Linear relationships were obtained over concentration ranges (5-50 μg/spot) for almotriptan and rizatriptan, and (5-60 μg/spot) for eletriptan. The second method based on the separation and determination of the studied drugs, using RP-HPLC technique. The separation was achieved on C18 Hypersil column, elution was carried out using phosphate buffer pH 3: methanol: acetonitrile (2: 1:1 v/v) at flow rate 2 mL/min and UV detection at 235 nm. Linear relationships were obtained over concentration ranges (10-200 μg/mL) for almotriptan and eletriptan, and (10-180 μg/mL) for rizatriptan. The chromatographic methods were successfully applied for the determination of each of the studied drugs in pure form, tablet form, and in laboratory prepared mixtures with their acid degradation products.
提出了两种稳定性指示色谱法,用于在存在酸降解产物的情况下测定阿莫曲坦、依来曲坦和利扎曲坦。第一种方法是定量密度薄层色谱法。展开系统分别为:对于阿莫曲坦,乙腈:甲醇:二氯甲烷:氨(10:6:3:1 v/v);对于依来曲坦,乙酸乙酯:甲醇:氨(15:4:1 v/v);对于利扎曲坦,甲醇:乙腈:氨(9:4:1 v/v)。薄层色谱板在235 nm处扫描。阿莫曲坦和利扎曲坦在浓度范围(5 - 50 μg/斑点)内、依来曲坦在浓度范围(5 - 60 μg/斑点)内获得线性关系。第二种方法基于使用反相高效液相色谱(RP - HPLC)技术分离和测定所研究的药物。在C18 Hypersil柱上实现分离,使用pH 3的磷酸盐缓冲液:甲醇:乙腈(2:1:1 v/v)以2 mL/min的流速进行洗脱,并在235 nm处进行紫外检测。阿莫曲坦和依来曲坦在浓度范围(10 - 200 μg/mL)内、利扎曲坦在浓度范围(10 - 180 μg/mL)内获得线性关系。这些色谱方法已成功应用于测定纯品、片剂形式以及与酸降解产物的实验室制备混合物中的每种所研究药物。