Tabani Hadi, Fakhari Ali Reza, Shahsavani Abolfath, Gharari Alibabaou Hossein
Department of Pure Chemistry, Faculty of Chemistry, Shahid Beheshti University, G.C., Evin, Tehran, Islamic Republic of Iran.
Chirality. 2014 May;26(5):260-7. doi: 10.1002/chir.22308. Epub 2014 Mar 17.
In this study, electromembrane extraction (EME) combined with cyclodextrin (CD)-modified capillary electrophoresis (CE) was applied for the extraction, separation, and quantification of propranolol (PRO) enantiomers from biological samples. The PRO enantiomers were extracted from aqueous donor solutions, through a supported liquid membrane (SLM) consisting of 2-nitrophenyl octyl ether (NPOE) impregnated on the wall of the hollow fiber, and into a 20-μL acidic aqueous acceptor solution into the lumen of hollow fiber. Important parameters affecting EME efficiency such as extraction voltage, extraction time, pH of the donor and acceptor solutions were optimized using a Box-Behnken design (BBD). Then, under these optimized conditions, the acceptor solution was analyzed using an optimized CD-modified CE. Several types of CD were evaluated and best results were obtained using a fused-silica capillary with ammonium acetate (80 mM, pH 2.5) containing 8 mM hydroxypropyl-β-CD as a chiral selector, applied voltage of 18 kV, and temperature of 20°C. The relative recoveries were obtained in the range of 78-95%. Finally, the performance of the present method was evaluated for the extraction and determination of PRO enantiomers in real biological samples.
在本研究中,电膜萃取(EME)结合环糊精(CD)修饰的毛细管电泳(CE)用于从生物样品中提取、分离和定量普萘洛尔(PRO)对映体。PRO对映体从供体水溶液中通过由浸渍在中空纤维壁上的2-硝基苯基辛基醚(NPOE)组成的支撑液膜(SLM),萃取到中空纤维内腔中的20 μL酸性水受体溶液中。使用Box-Behnken设计(BBD)优化了影响EME效率的重要参数,如萃取电压、萃取时间、供体和受体溶液的pH值。然后,在这些优化条件下,使用优化的CD修饰CE对受体溶液进行分析。评估了几种类型的CD,使用含有8 mM羟丙基-β-CD作为手性选择剂、施加电压为18 kV、温度为20°C的醋酸铵(80 mM,pH 2.5)的熔融石英毛细管获得了最佳结果。相对回收率在78-95%范围内。最后,评估了本方法在实际生物样品中提取和测定PRO对映体的性能。