聚多巴胺修饰的纳米/亚微米二氧化钛纤维涂层高效固相微萃取邻苯二甲酸酯类化合物  

Polydopamine Modified Titanium Dioxide Nano/Submicro Particles Coating for Solid Phase Microextraction of Phthalic Acid Esters

作　　者：王会菊 沈小燕 李康 王守佳 马玉龙 WANG Hui-ju;SHEN Xiao-yan;LI Kang;WANG Shou-jia;MA Yu-long(College of Chemistry and Chemical Engineering,Qinghai Minzu University,Xining 810007,China;Key Lab of Resource Chemistry&Eco-environmental Protection in Qinghai-Tibet Plateau,State Ethnic Affairs Committee,Qinghai Minzu University,Xining 810007,China)

机构地区：[1]青海民族大学化学化工学院,青海西宁810007 [2]青海民族大学、青藏高原资源化学与生态环境保护国家民委重点实验室,青海西宁810007

出　　处：《分析测试学报》2023年第4期480-487,共8页Journal of Instrumental Analysis

基　　金：国家自然科学基金项目(22166029);青海民族大学校级规划项目(2021XJGH13)。

摘　　要：采用电泳沉积与自聚合方法在镍钛(NiTi)合金表面组装聚多巴胺(PDA)修饰的纳米/亚微米二氧化钛(PDA@TiO2NPs)固相微萃取(SPME)纤维涂层。电泳沉积前,先将NiTi合金水热处理原位生成氧化钛和氧化镍复合纳米片(TiO2NiOCNFs@NiTi),使涂层与NiTi合金牢固结合。将制备的PDA@TiO2NPs@TiO2NiOCNFs@NiTi纤维与高效液相色谱(HPLC)联用,用于富集、萃取和测定环境水样中的5种邻苯二甲酸酯(PAEs)类有机污染物,并考察了影响萃取效率的主要因素。在优化条件下,采用外标法对方法学参数进行评价。结果显示,5种PAEs在0.1~200μg/L范围内呈良好的线性关系,相关系数(r)不小于0.9989,检出限(LOD)和定量下限(LOQ)分别为0.013~0.055μg/L和0.043~0.18μg/L。单支纤维在日内和日间对50μg/L PAEs标准溶液萃取测定的相对标准偏差(RSD)分别为5.4%~6.8%和5.7%~7.0%。该方法成功用于实际水样中痕量PAEs的测定,加标回收率为87.8%~102%,RSD不大于8.2%。该方法灵敏度高、准确度好,适用于不同环境水样中痕量PAEs的高效分析测定。A new polydopamine modified titanium dioxide nano/submicro particles coating(PDA@TiO2NPs)was fabricated on the NiTi alloy wire by electrophoretic deposition and self-polymerization modification in this paper.Prior to electrophoretic deposition,the titanium and nickel oxide composite nanoflakes(TiO2NiOCNFs)were in situ grown on NiTi alloy wire via hydrothermal treatment in order to boost the binding strength between TiO2NPs coating and NiTi fiber.Coupled with high performance liquid chro⁃matography(HPLC),the fabricated PDA@TiO2NPs@TiO2NiOCNFs@NiTi fiber was applied as a solid phase microextraction(SPME)fiber to the determination of 5 phthalic acid esters(PAEs)in water sam⁃ples.The main parameters affecting extraction efficiency such as extraction temperature,extraction time,stirring rate and ion strength were investigated and optimized.Under the optimized conditions,the analytical parameters including linear ranges,recoveries,limits of detection(LODs)and limits of quantitation(LOQs)were investigated and evaluated by external standard method.The results showed that the proposed method showed good linearity in the range of 0.1-200μg/L,with correlation coeffi⁃cients(r)not less than 0.9989.LODs and LOQs were in the range of 0.013-0.055μg/L and 0.043-0.18μg/L,respectively.The intra-day and inter-day relative standard deviations(RSDs)for each fiber ranged from 5.4%to 6.8%and 5.7%to 7.0%,respectively.Moreover,the developed method was successfully used to extract and detect trace PAEs in real water samples.The spiked recov⁃eries for target PAEs in real water samples ranged from 87.8%to 102%,with RSDs not more than 8.2%.In addition,the established method has high sensitivity,good accuracy,which was suitable for the high efficient detection of PAEs in different environmental water samples.

关 键 词：聚多巴胺 电泳沉积 纳米/亚微米二氧化钛 固相微萃取 高效液相色谱 邻苯二甲酸酯 

分 类 号：O657.72[理学—分析化学] TQ314.257[理学—化学]