Du Junliang, Li Juan, Lv Rui, Du Xinzhen
College of Chemistry and Chemical Engineering, Mianyang Normal University Mianyang 621000 China.
College of Chemistry and Chemical Engineering, Northwest Normal University Lanzhou 730070 China
RSC Adv. 2022 Apr 19;12(19):11933-11941. doi: 10.1039/d2ra01031c. eCollection 2022 Apr 13.
The nature and fabrication of fiber coatings with good adsorption capacity and selectivity play a decisive role in solid-phase microextraction (SPME). In this work, a novel SPME fiber was fabricated through hydrothermal growth of octahedral TiO nanoparticles (TiONPs) on a superelastic nickel/titanium alloy (NiTi) wire substrate in acid solution. The resulting fiber coatings were characterized by scanning electron microscopy and energy dispersive X-ray spectroscopy. Acid types, acid concentration as well as hydrothermal temperature and time were found to be effective route to manipulate the morphologies and composition of TiO-based nanoflakes grown on the NiTi fiber substrates. At the concentration of 0.4 mol L HCl as well as hydrothermal temperature of 150 °C and hydrothermal time of 12 h, TiONPs were grown on the NiTi wire substrates. The obtained NiTi wire with the TiONPs coating (NiTi@TiONPs fiber) was employed to investigate the adsorption of some representative aromatic analytes in water samples coupling with high-performance liquid chromatography with UV detection (HPLC/UV). The results clearly demonstrate that the fiber exhibits good extraction selectivity for ultraviolet filters (UVFs). In view of good extraction selectivity for the selected UVFs, the key experimental parameters were optimized. Under the optimum conditions, the calibration curves were linear in the ranges of 0.05-100 μg L with the correlation coefficients greater than 0.998. Limits of detection (LODs) were 0.007 to 0.064 μg L. Furthermore, the intra-day and inter-day repeatability of the proposed method with the single fiber varied from 4.3% to 6.1% and from 4.5% to 6.8%, respectively. The fiber-to-fiber reproducibility ranged from 5.8% to 8.2%. The developed SPME-HPLC/UV method was applied to selective preconcentration and sensitive determination of target UVFs from real water samples. Moreover, the fabricated fiber showed precisely controllable growth and 150 extraction and desorption cycles.
具有良好吸附容量和选择性的纤维涂层的性质与制备在固相微萃取（SPME）中起着决定性作用。在本工作中，通过在酸性溶液中于超弹性镍钛合金（NiTi）丝基底上水热生长八面体TiO纳米颗粒（TiONPs），制备了一种新型SPME纤维。通过扫描电子显微镜和能量色散X射线光谱对所得纤维涂层进行了表征。发现酸的类型、酸浓度以及水热温度和时间是控制在NiTi纤维基底上生长的TiO基纳米片的形貌和组成的有效途径。在0.4 mol L HCl浓度、150℃水热温度和12 h水热时间条件下，TiONPs生长在NiTi丝基底上。将获得的带有TiONPs涂层的NiTi丝（NiTi@TiONPs纤维）用于结合高效液相色谱-紫外检测（HPLC/UV）研究水样中一些代表性芳香族分析物的吸附。结果清楚地表明，该纤维对紫外线过滤剂（UVFs）表现出良好的萃取选择性。鉴于对所选UVFs具有良好的萃取选择性，对关键实验参数进行了优化。在最佳条件下，校准曲线在0.05 - 100 μg L范围内呈线性，相关系数大于0.998。检测限（LODs）为0.007至0.064 μg L。此外，单根纤维所提方法的日内和日间重复性分别为4.3%至6.1%和4.5%至6.8%。纤维间的重现性为5.8%至8.2%。所开发的SPME - HPLC/UV方法用于实际水样中目标UVFs的选择性预富集和灵敏测定。此外，所制备的纤维显示出精确可控的生长以及150次萃取和解吸循环。
