Department of Chemistry, Shahid Beheshti University, G.C., Tehran 1983963113, Iran.
J Chromatogr A. 2013 Sep 20;1308:25-31. doi: 10.1016/j.chroma.2013.07.088. Epub 2013 Jul 29.
A simple, rapid, and efficient method, based on surfactant assisted dispersive liquid-liquid microextraction (SA-DLLME), followed by high performance liquid chromatography (HPLC) has been developed for simultaneous preconcentration and trace detection of zonisamide and carbamazepine in biological samples. A conventional cationic surfactant called cethyltrimethyl ammonium bromide (CTAB) was used as a disperser agent in the proposed approach. 1.5 mL of CTAB (0.45 mmol L(-1)) (disperser solvent) containing 50.0 μL of 1-octanol (extraction solvent) was injected rapidly into the 7.0 mL of water or diluted plasma or urine. A cloudy solution (water, 1-octanol, and CTAB) was formed in the test tube. After formation of cloudy solution, the mixture was centrifuged and 20 μL of collected phase was injected into HPLC for subsequent analysis. Some parameters such as the type and volume of the extraction solvent, the type and concentration of surfactant, pH, ionic strength and centrifugation time were evaluated and optimized. Under optimum extraction conditions, the limits of detections (LODs) were 2.1 and 1.5 μg L(-1) (based on 3Sb/m) for urine samples, and 2.3 and 1.6 μg L(-1) for plasma samples. Linear dynamic range of 5-300 and 5-200 μg L(-1) were obtained for zonisamide and carbamazepine in all samples. Finally, the applicability of the proposed method was evaluated by extraction and determination of the drugs in urine and plasma samples.
一种基于表面活性剂辅助分散液液微萃取(SA-DLLME)结合高效液相色谱(HPLC)的简单、快速、高效的方法已被开发用于同时预浓缩和痕量检测生物样品中的佐米曲坦和卡马西平。在提出的方法中,使用了一种常规的阳离子表面活性剂称为十六烷基三甲基溴化铵(CTAB)作为分散剂。将 1.5 mL 的 CTAB(0.45 mmol L(-1))(分散溶剂)和 50.0 μL 的 1-辛醇(萃取溶剂)快速注入 7.0 mL 的水或稀释的血浆或尿液中。在试管中形成浑浊溶液(水、1-辛醇和 CTAB)。形成浑浊溶液后,将混合物离心,用 20 μL 收集的相注入 HPLC 进行后续分析。评估并优化了一些参数,例如萃取溶剂的类型和体积、表面活性剂的类型和浓度、pH 值、离子强度和离心时间。在最佳萃取条件下,对尿液样品的检测限(LOD)分别为 2.1 和 1.5 μg L(-1)(基于 3Sb/m),对血浆样品的检测限分别为 2.3 和 1.6 μg L(-1)。在所有样品中,佐米曲坦和卡马西平的线性动态范围分别为 5-300 和 5-200 μg L(-1)。最后,通过在尿液和血浆样品中提取和测定药物来评估所提出方法的适用性。