Belal F, Ibrahim F, Sheribah Z A, Alaa H
Department of pharmaceutical analytical chemistry, faculty of pharmacy, Mansoura university, 35516 Mansoura, Egypt.
Department of pharmaceutical analytical chemistry, faculty of pharmacy, Mansoura university, 35516 Mansoura, Egypt.
Ann Pharm Fr. 2018 May;76(3):172-186. doi: 10.1016/j.pharma.2018.02.003. Epub 2018 Mar 22.
This work describes a micellar liquid chromatographic method which was developed and validated to determine simultaneously three structurally-related antiepileptic drugs; namely carbamazepine (CMZ), oxcarbazepine (OCZ) and eslicarbazepine acetate (ECZ). The analysis was achieved using a phenyl column (250mm×4.6mm i.d., 5μm particle size), a mobile phase consisting of a mixture of 0.3% triethylamine and 10% n-butanol in a solution of 0.05M sodium dodecyl sulphate adjusted to pH 7.0 using 0.02M orthophosphoric acid. The mobile phase was pumped at a flow rate of 1.5mLmin and detection was adjusted at 215nm. The method showed good linearity (r>0.998) over the concentration ranges of 0.1-10 for CMZ and OCZ and 0.2-20μgmL for ECZ. The suggested method was successfully applied for the analysis of the studied drugs in their dosage forms and for the determination of CMZ and OCZ in spiked human urine and plasma without prior extraction. The proposed method was further extended to the analysis of real samples of plasma and urine of volunteers receiving therapy of CMZ and OCZ. Furthermore, the method was successfully applied to tablets dissolution-rate testing, and the results were satisfactory.
本研究描述了一种胶束液相色谱法，该方法经过开发和验证，可同时测定三种结构相关的抗癫痫药物，即卡马西平（CMZ）、奥卡西平（OCZ）和醋酸艾司利卡西平（ECZ）。分析采用苯基柱（250mm×4.6mm内径，5μm粒径），流动相由0.3%三乙胺和10%正丁醇在0.05M十二烷基硫酸钠溶液中混合而成，用0.02M正磷酸调节pH至7.0。流动相以1.5mL/min的流速泵送，检测波长设定为215nm。该方法在CMZ和OCZ的浓度范围为0.1 - 10μg/mL以及ECZ的浓度范围为0.2 - 20μg/mL时显示出良好的线性（r>0.998）。所建议的方法成功应用于所研究药物剂型的分析，以及在未经预先萃取的情况下测定加标的人尿液和血浆中的CMZ和OCZ。该方法进一步扩展到接受CMZ和OCZ治疗的志愿者血浆和尿液实际样品的分析。此外，该方法成功应用于片剂溶出度测试，结果令人满意。
