Yaripour Saeid, Mohammadi Ali, Esfanjani Isa, Walker Roderick B, Nojavan Saeed
Department of Drug and Food Control, Faculty of Pharmacy, Tehran University of Medical Sciences, Tehran, Iran.
Department of Pharmaceutical and Food Control, Faculty of Pharmacy, Urmia University of Medical Sciences, Urmia, Iran.
EXCLI J. 2018 Apr 23;17:349-361. doi: 10.17179/excli2018-1140. eCollection 2018.
In this study, for the first time, an electro-driven microextraction method named electromembrane extraction combined with a simple high performance liquid chromatography and ultraviolet detection was developed and validated for the quantitation of zolpidem in biological samples. Parameters influencing electromembrane extraction were evaluated and optimized. The membrane consisted of 2-ethylhexanol immobilized in the pores of a hollow fiber. As a driving force, a 150 V electric field was applied to facilitate the analyte migration from the sample matrix to an acceptor solution through a supported liquid membrane. The pHs of donor and acceptor solutions were optimized to 6.0 and 2.0, respectively. The enrichment factor was obtained >75 within 15 minutes. The effect of carbon nanotubes (as solid nano-sorbents) on the membrane performance and EME efficiency was evaluated. The method was linear over the range of 10-1000 ng/mL for zolpidem (R >0.9991) with repeatability ( %RSD) between 0.3 % and 7.3 % ( = 3). The limits of detection and quantitation were 3 and 10 ng/mL, respectively. The sensitivity of HPLC-UV for the determination of zolpidem was enhanced by electromembrane extraction. Finally, the method was employed for the quantitation of zolpidem in biological samples with relative recoveries in the range of 60-79 %.
在本研究中，首次开发并验证了一种名为电膜萃取的电驱动微萃取方法，该方法结合了简单的高效液相色谱法和紫外检测，用于生物样品中唑吡坦的定量分析。对影响电膜萃取的参数进行了评估和优化。该膜由固定在中空纤维孔中的2-乙基己醇组成。作为驱动力，施加150 V的电场以促进分析物通过支撑液膜从样品基质迁移到接受液中。供体溶液和接受液的pH值分别优化为6.0和2.0。在15分钟内富集因子大于75。评估了碳纳米管（作为固体纳米吸附剂）对膜性能和电膜萃取效率的影响。该方法对唑吡坦在10-1000 ng/mL范围内呈线性（R>0.9991），重复性（%RSD）在0.3%至7.3%之间（n = 3）。检测限和定量限分别为3和10 ng/mL。电膜萃取提高了高效液相色谱-紫外法测定唑吡坦的灵敏度。最后，该方法用于生物样品中唑吡坦的定量分析，相对回收率在60-79%范围内。
