Tajik Mohammad, Yamini Yadollah, Esrafili Ali, Ebrahimpour Behnam
Department of Chemistry, Faculty of Sciences, Tarbiat Modares University, P.O. Box 14115-175, Tehran, Iran.
Department of Chemistry, Faculty of Sciences, Tarbiat Modares University, P.O. Box 14115-175, Tehran, Iran.
J Pharm Biomed Anal. 2015 Mar 25;107:24-31. doi: 10.1016/j.jpba.2014.12.028. Epub 2014 Dec 23.
In this research, a rapid efficient and automated instrument based on hollow fiber liquid-phase microextraction (HF-LPME) followed by high performance liquid chromatography (HPLC) with UV-vis detection was applied for the preconcentration and determination of two hormonal drugs (megestrol acetate and levonorgestrel) in water and urinary samples. n-Dodecane was used as the supported liquid membrane (SLM) and methanol was used as the acceptor phase in the hollow fiber lumen. The effects of different parameters such as fiber length, extraction time, stirring rate, and ionic strength on the extraction efficiency were investigated using modified simplex and central composite design as the screening and optimization methods, respectively. The composition effect of SLM and type of acceptor phase were optimized separately. For adjustment of the SLM composition, trioctylphosphine oxide (TOPO) was chosen. Under optimized condition, the calibration curves were linear (r(2)>0.997) in the range of 0.5-200 μg L(-1). LOD for both of the drugs were 0.25 μg L(-1). The applicability of this technique was examined by analyzing drugs in water and urine samples. The relative recoveries of the drugs were in the range of 86.2-102.3% that show the capability of the method for the determination of the drugs in various matrices.
在本研究中，一种基于中空纤维液相微萃取（HF-LPME），随后采用高效液相色谱（HPLC）并结合紫外可见检测的快速、高效且自动化的仪器，被应用于水和尿液样本中两种激素类药物（醋酸甲地孕酮和左炔诺孕酮）的预浓缩和测定。正十二烷用作支撑液膜（SLM），甲醇用作中空纤维内腔中的接受相。分别采用改进单纯形法和中心复合设计作为筛选和优化方法，研究了纤维长度、萃取时间、搅拌速率和离子强度等不同参数对萃取效率的影响。分别对支撑液膜的组成效应和接受相类型进行了优化。为调整支撑液膜的组成，选择了三辛基氧化膦（TOPO）。在优化条件下，校准曲线在0.5 - 200 μg L⁻¹范围内呈线性（r²>0.997）。两种药物的检测限均为0.25 μg L⁻¹。通过分析水和尿液样本中的药物来检验该技术的适用性。药物的相对回收率在86.2 - 102.3%范围内，表明该方法具有测定各种基质中药物的能力。
