Gumustas Mehmet, Caglayan Mehmet Gokhan, Onur Feyyaz, Ozkan Sibel A
Faculty of Arts & Sciences, Department of Chemistry, Hitit University, Corum, Turkey.
Ankara University, Faculty of Pharmacy, Department of Analytical Chemistry, Ankara, Turkey.
Biomed Chromatogr. 2018 Apr;32(4). doi: 10.1002/bmc.4158. Epub 2018 Jan 9.
A combination of antiretroviral agents is frequently used in effective treatment of the human immunodeficiency virus infection. In this study, two different separation methods are presented for the simultaneous determination of emtricitabine, rilpivirine and tenofovir from raw materials and urine samples. Developed liquid chromatography and capillary electrophoresis methods were thoroughly optimized for high analytical performances. Optimization of multiple variables at the same time by performing a minimum number of experiments was achieved by the Box-Behnken design, which is an experimental design in response surface methodology, in capillary electrophoresis. The results of the experimental design ensure minimum analysis time with well-separated analytes. Separation conditions, such as different stationary phases, pH level, organic modifiers and temperatures in liquid chromatography method, were also optimized. In particular, among stationary phases, the core-shell column especially enhanced the effectiveness of separation in liquid chromatography. Both methods were fully validated and applied to real samples. The main advantage of the developed methods is the separation of the drug combination in a short time with high efficiency and without any time-consuming steps.
抗逆转录病毒药物组合常用于有效治疗人类免疫缺陷病毒感染。在本研究中，提出了两种不同的分离方法，用于同时测定原料和尿液样本中的恩曲他滨、利匹韦林和替诺福韦。所开发的液相色谱法和毛细管电泳法针对高分析性能进行了全面优化。通过Box-Behnken设计实现了在毛细管电泳中通过最少的实验同时优化多个变量，Box-Behnken设计是响应面法中的一种实验设计。实验设计的结果确保了分析时间最短且分析物分离良好。液相色谱法中的分离条件，如不同的固定相、pH值、有机改性剂和温度等也进行了优化。特别是在固定相中，核壳柱尤其提高了液相色谱中的分离效果。两种方法均经过充分验证并应用于实际样品。所开发方法的主要优点是能在短时间内高效分离药物组合，且无需任何耗时步骤。
