Radwan Mahasen A, Abdine Heba H, Aboul-Enein Hassan Y
Department of Clinical Pharmacy, College of Pharmacy, King Saud University, and Centre for Clinical Research, King Faisal Specialist Hospital and Research Centre, Riyadh 11495, Saudi Arabia.
Biomed Chromatogr. 2006 Feb;20(2):211-6. doi: 10.1002/bmc.556.
A new, precise, simple and accurate HPLC method was developed for the first time to separate and determine mebeverine enantiomers. Enantiomeric resolution was achieved on a cellulose Tris (3,5-dimethylphenyl carbamate) column known as Chiralcel OD, with UV detection at 263 nm. The mobile phase consisted of n-hexane, isopropyl alcohol and triethylamine (90:9.9:0.1 v/v/v). Sample run time was 18 min. On using the chromatographic conditions described, mebeverine enantiomers were well resolved with mean retention times of about 11 and 14 min. A linear response (r>0.999) was observed over the concentration range 0.5-20 microg/mL racemic mebeverine. Precision, accuracy and stability were studied according to ICH guidelines. The limit of detection was found to be 0.05 microg/mL for each enantiomer of mebeverine. The proposed method was applied for analysis of mebeverine in commercially available tablets dosage formulations. Examples of application to biological samples are also given. Reanalysis of samples several weeks after the initial analysis showed no degradation of mebeverine.
首次开发了一种新的、精确、简单且准确的高效液相色谱法来分离和测定美贝维林对映体。在一种名为Chiralcel OD的纤维素三（3,5 - 二甲基苯基氨基甲酸酯）柱上实现了对映体拆分，采用263 nm波长的紫外检测。流动相由正己烷、异丙醇和三乙胺（90:9.9:0.1 v/v/v）组成。样品运行时间为18分钟。在所述色谱条件下，美贝维林对映体得到了很好的分离，平均保留时间约为11分钟和14分钟。在0.5 - 20 μg/mL外消旋美贝维林浓度范围内观察到线性响应（r>0.999）。根据国际人用药品注册技术协调会（ICH）指南研究了精密度、准确度和稳定性。发现美贝维林每种对映体的检测限为0.05 μg/mL。所提出的方法应用于市售片剂剂型中美贝维林的分析。还给出了应用于生物样品的示例。在初始分析几周后对样品进行重新分析表明美贝维林没有降解。
