Environmental and Bio-Analytical Laboratories, Department of Chemistry, Sharif University of Technology, P.O. Box 11365-9516, Tehran, Iran.
Environmental and Bio-Analytical Laboratories, Department of Chemistry, Sharif University of Technology, P.O. Box 11365-9516, Tehran, Iran.
J Chromatogr A. 2018 Nov 2;1574:18-26. doi: 10.1016/j.chroma.2018.08.055. Epub 2018 Aug 31.
In this study, cellulose acetate (CA) fibers were prepared using different solvent systems in electrospinning. The recorded scanning electron microscopy micrographs indicated that the morphology of the prepared fibers is closely associated with the type of electrospinning solvents. The prepared CA fibers were used as an extractive phase for on-line micro-solid phase extraction (μ-SPE) of nonsteroidal-inflammatory drugs (NSAIDs) in biological samples pursued by HPLC-UV determination. Work conducted on this research ascertained that the use of dichloromethane:acetone (3:1, v/v) solvent system in the CA dissolution for electrospinning, leads to the formation of porous ribbon-like fibers and subsequent excellent extraction efficiencies for the selected drugs. Moreover, the effects of diverse parameters on the extraction efficiency were surveyed and optimized. The proposed method was used for determination of naproxen, diclofenac and mefenamic acid in human urine and plasma samples. The optimized method was validated and the limits of detection (1.0-2.4 μg L), limits of quantification (3.3-8.0 μg L) and linear dynamic range (4.0-1000.0 μg L) were obtained. The reproducibility (relative standard deviation: 2.6-7.9%) was in an acceptable range. Trueness of the procedure was accomplished through recovery assays in urine (94-105%) and plasma (85-102%) samples, indicating the minor contribution from the sample matrix. Finally, the CA porous fibers within the framework of the μ-SPE method were found to be appropriate for the separation and determination of the selected drugs in urine and plasma samples collected from treated patients. Also, the adsorption behavior of the porous fibers was well described by Freundlich isotherm and porous fibers showed acceptable adsorption capacity.
在这项研究中,采用不同的溶剂体系在静电纺丝中制备醋酸纤维素(CA)纤维。记录的扫描电子显微镜照片表明,所制备纤维的形态与静电纺丝溶剂的类型密切相关。将制备的 CA 纤维用作生物样品中非甾体抗炎药(NSAIDs)的在线微固相萃取(μ-SPE)的萃取相,通过 HPLC-UV 测定进行。该研究工作证实,在 CA 溶解于用于静电纺丝的二氯甲烷:丙酮(3:1,v/v)溶剂系统中,形成多孔带状纤维,随后对所选药物具有优异的萃取效率。此外,还研究并优化了各种参数对萃取效率的影响。该方法用于测定人尿和血浆样品中的萘普生、双氯芬酸和甲芬那酸。优化后的方法经过验证,检测限(1.0-2.4μg L)、定量限(3.3-8.0μg L)和线性动态范围(4.0-1000.0μg L)。重现性(相对标准偏差:2.6-7.9%)在可接受范围内。通过尿(94-105%)和血浆(85-102%)样品中的回收测定验证了该程序的准确性,表明样品基质的贡献较小。最后,在μ-SPE 方法的框架内,CA 多孔纤维适用于从治疗患者采集的尿和血浆样品中分离和测定所选药物。此外,多孔纤维的吸附行为很好地用 Freundlich 等温线描述,并且多孔纤维表现出可接受的吸附能力。