镍钛合金纤维基体上氧化锌纳米片的电沉积及其对环境水样中紫外线吸收剂的高效固相微萃取  

Electrodeposition of zinc oxide nanosheets on nickel/titanium alloy fibers for highly efficient solid phase microextraction of ultraviolet filters in environmental water

作　　者：杜稼健 王会菊[1] 王雪梅[1] 杜新贞[1] 卢小泉[1] DU Jia-jian;WANG Hui-ju;WANG Xue-mei;DU Xin-zhen;LU Xiao-quan(College of Chemistry and Chemical Engineering, Northwest Normal University, Lanzhou 73007)

机构地区：[1]西北师范大学化学化工学院,兰州730070

出　　处：《分析试验室》2018年第5期497-502,共6页Chinese Journal of Analysis Laboratory

基　　金：国家自然科学基金项目(21265019)资助

摘　　要：以镍钛合金(NiTi)丝为固相微萃取(SPME)纤维基体,采用水热法原位生长网状交联钛/镍复合氧化物纳米片(TiO_2/NiOCNSs),随后通过电化学沉积,将氧化锌纳米片(ZnONSs)可控组装在NiTi-TiO_2/NiOCNSs纤维上。与HPLC联用,考察所组装NiTi-TiO_2/NiOCNSs@ZnONSs纤维对水样中痕量紫外线吸收剂的吸附性能,优化实验条件,建立了SPME-HPLC测定方法。在0.05~200μg/L范围内具有良好线性关系(相关系数>0.999),检出限为0.009~0.065μg/L;该法的单根纤维日内测量相对标准偏差(RSDs)为4.6%~5.5%,日间测量RSDs为5.4%~6.8%,该法的5根不同批次所组装纤维RSDs为6.7%~7.9%。实际水样分析结果表明,加标回收率为86.8%~105.9%。所组装NiTi基纤维具有良好制备重现性和很长的使用寿命,一根纤维可完成整个分析过程和批量样品的测量。所建立方法适用于不同类型环境水样中痕量紫外线吸收剂的富集分离和灵敏测定。Hydrothermal treatment was used for the in situ growth of net-like cross-linked TiO2/Ni OCNSs on the nickel/titanium alloy（ NiTi） wire as a fiber substrate for solid-phase microextraction（ SPME）. Subsequently controllable fabrication of zinc oxide nanosheets（ Zn ONSs） coating was carried out on the Ni Ti fiber with titanium and nickel oxide composite nanosheets（ NiTi-TiO2/NiCNSs）. The SPME performance of the fabricated fiber was investigated for concentration and determination of ultraviolet（ UV） filters coupled to HPLC with UV detection（ HPLC-UV）. The main parameters affecting extraction performance were investigated and optimized. Under the optimized conditions,the calibration graphs were linear over the range 0. 05 ～ 200 μg/L. The limits of detection of the proposed method were 0. 09 ～ 0. 065 μg/L. The intra-day and inter-day repeatability of single fiber was 4. 6% ～ 5. 5% and 5. 4% ～ 6. 8%, respectively, and the fiber-to-fiber reproducibility 6. 7% ～ 7. 9% for the extraction of spiking water with 50 μg/L each analytes（ n = 5）.The experimental results demonstrated that the relative recoveries of target UV filters from real environmental water samples were in the range of 86. 8% ～ 105. 9%. Moreover,this Ni Ti-based fiber could be fabricated in a highly reproducible manner and has long lifetime. A single fiber iscompetent for all of the analyses in the entire sample sequence. The established method is suitable for the concentration and the sensitive determination of trace UV filters in different environmental water samples.

关 键 词：镍钛氧化物复合纳米片 氧化锌纳米片 紫外线吸收剂 固相微萃取 

分 类 号：X830.2[环境科学与工程—环境工程]