Asadi Mohammad, Dadfarnia Shayessteh, Haji Shabani Ali Mohammad, Abbasi Bijan
Department of Chemistry, Faculty of Science, Yazd University, Yazd, Iran.
Khorassan Research Institute for Food Science and Technology, Mashhad, Iran.
J Sep Sci. 2015 Jul;38(14):2510-6. doi: 10.1002/jssc.201500237. Epub 2015 Jun 8.
A novel and simple method based on solidified floating organic drop microextraction followed by high-performance liquid chromatography with ultraviolet detection has been developed for simultaneous preconcentration and determination of phenobarbital, lamotrigine, and phenytoin in human plasma and urine samples. Factors affecting microextraction efficiency such as the type and volume of the extraction solvent, sample pH, extraction time, stirring rate, extraction temperature, ionic strength, and sample volume were optimized. Under the optimum conditions (i.e. extraction solvent, 1-undecanol (40 μL); sample pH, 8.0; temperature, 25°C; stirring rate, 500 rpm; sample volume, 7 mL; potassium chloride concentration, 5% and extraction time, 50 min), the limits of detection for phenobarbital, lamotrigine, and phenytoin were 1.0, 0.1, and 0.3 μg/L, respectively. Also, the calibration curves for phenobarbital, lamotrigine, and phenytoin were linear in the concentration range of 2.0-300.0, 0.3-200.0, and 1.0-200.0 μg/L, respectively. The relative standard deviations for six replicate extractions and determinations of phenobarbital, lamotrigine, and phenytoin at 50 μg/L level were less than 4.6%. The method was successfully applied to determine phenobarbital, lamotrigine, and phenytoin in plasma and urine samples.
已开发出一种基于固化浮动有机滴微萃取,随后进行高效液相色谱-紫外检测的新颖且简单的方法,用于同时预富集和测定人血浆和尿液样本中的苯巴比妥、拉莫三嗪和苯妥英。对影响微萃取效率的因素进行了优化,如萃取溶剂的类型和体积、样品pH值、萃取时间、搅拌速率、萃取温度、离子强度和样品体积。在最佳条件下(即萃取溶剂为1-十一醇(40 μL);样品pH值为8.0;温度为25°C;搅拌速率为500 rpm;样品体积为7 mL;氯化钾浓度为5%;萃取时间为50分钟),苯巴比妥、拉莫三嗪和苯妥英的检测限分别为1.0、0.1和0.3 μg/L。此外,苯巴比妥、拉莫三嗪和苯妥英的校准曲线在浓度范围分别为2.0 - 300.0、0.3 - 200.0和1.0 - 200.0 μg/L时呈线性。在50 μg/L水平下,对苯巴比妥、拉莫三嗪和苯妥英进行六次重复萃取和测定的相对标准偏差小于4.6%。该方法已成功应用于测定血浆和尿液样本中的苯巴比妥、拉莫三嗪和苯妥英。