Bagheri Habib, Piri-Moghadam Hamed, Rastegar Soroush, Taheri Navid
Environmental and Bio-Analytical Laboratories, Department of Chemistry, Sharif University of Technology, Tehran, Iran.
J Sep Sci. 2014 Aug;37(15):1982-8. doi: 10.1002/jssc.201400252. Epub 2014 Jun 10.
Titanium(IV) tetraisopropoxide was employed as a metal oxide sol-gel precursor to prepare ceramic composite nanofibers by the electrospinning system. To facilitate this process and obtain the desired nanofibers with higher aspect ratios and surface area, poly(vinylpyrrolidone) was added to the sol of titania. Four ceramic nanofibers sheets based on titania were prepared while each sheet contained different transition metals such as Fe-Mn, Fe-Ni, Fe-Co, and Fe-Mn-Co-Ni. The scanning electron microscope images showed good homogeneity for all the prepared ceramic composites with a diameter range of 100-250 nm. The sorption efficiency was investigated by a micro-solid-phase extraction setup in online combination with high-performance liquid chromatography for the determination of naproxen and clobetasol. All the prepared composites exhibited comparable efficiencies for the desired analytes and the type of metal showed insignificant effect. For the selected composite with Fe-Mn, the linearity of the analytes was in the range of 1-1000 μg/L and the limit of detection values were found to be 2 and 0.3 μg/L for naproxen and clobetasol, respectively. The developed method was extended to the analysis of urine and blood plasma samples and acceptable relative standard deviations were obtained at two concentration levels.
采用四异丙醇钛作为金属氧化物溶胶 - 凝胶前驱体，通过静电纺丝系统制备陶瓷复合纳米纤维。为促进该过程并获得具有更高长径比和表面积的所需纳米纤维，将聚乙烯吡咯烷酮添加到二氧化钛溶胶中。制备了四种基于二氧化钛的陶瓷纳米纤维片，每片含有不同的过渡金属，如铁 - 锰、铁 - 镍、铁 - 钴以及铁 - 锰 - 钴 - 镍。扫描电子显微镜图像显示，所有制备的陶瓷复合材料均具有良好的均匀性，直径范围为100 - 250纳米。通过微固相萃取装置与高效液相色谱在线联用，研究了对萘普生和氯倍他索的吸附效率。所有制备的复合材料对所需分析物表现出相当的效率，金属类型的影响不显著。对于所选的铁 - 锰复合材料，分析物的线性范围为1 - 1000μg/L，萘普生和氯倍他索的检测限分别为2μg/L和0.3μg/L。所开发的方法扩展到尿液和血浆样品的分析，并在两个浓度水平获得了可接受的相对标准偏差。
