Department of Analytical Chemistry, Faculty of Chemistry, Urmia University, Urmia, Iran.
J Pharm Biomed Anal. 2013 Nov;85:283-7. doi: 10.1016/j.jpba.2013.07.025. Epub 2013 Aug 3.
A novel analytical method based on the use of a modified dispersive liquid-liquid microextraction (DLLME) technique by ionic liquids has been developed for the first time. This method was applied for the determination of salmeterol in dried blood spot samples from asthmatic patients followed by HPLC system equipped with fluorescence detector. The main novelty of the present work deals with the analysis of salmeterol in dried blood spot with significant advantages with regard to invasive sampling, volume of blood used (<20 μL), storage and transport of biological materials and requirements for special biohazard arrangements. The effects of significant factors in microextraction procedure including extracting and disperser solvents volume, sample pH and salt contents were investigated. Under optimized conditions, the mean recoveries were higher than 90.0% with linear responses about 1.00-500 ng mL(-1) concentration range. The limit of detection (LOD) was 0.30 ng mL(-1) in S/N of 3. Intra-day (n=6) and inter-day (n=3) assay precision showed relative standard deviation lower than 6.0 and 8.5% for studied drug, respectively. The developed microextraction procedure was simpler and faster than conventional extraction techniques and was omitted hazard organic solvents. Finally, the proposed method is suitable for the analysis of salmeterol in dried blood spots from asthmatic patients for therapeutic drug monitoring purpose.
首次开发了一种基于离子液体改进型分散液液微萃取（DLLME）技术的新型分析方法。该方法应用于哮喘患者干血斑样品中沙美特罗的测定，随后采用配备荧光检测器的 HPLC 系统。本工作的主要新颖之处在于分析干血斑中的沙美特罗，与侵入性采样、使用的血量（<20 μL）、生物材料的储存和运输以及特殊生物危害处理要求相比具有显著优势。研究了微萃取过程中的重要因素，包括萃取和分散溶剂体积、样品 pH 值和盐含量。在优化条件下，平均回收率高于 90.0%，浓度范围为 1.00-500ng mL(-1)。在 S/N 为 3 时，检测限（LOD）为 0.30ng mL(-1)。日内（n=6）和日间（n=3）测定精密度分别显示研究药物的相对标准偏差低于 6.0%和 8.5%。与传统萃取技术相比，所开发的微萃取程序更简单、更快，且无需使用危险有机溶剂。最后，该方法适用于哮喘患者干血斑中沙美特罗的分析，可用于治疗药物监测目的。
