钛丝原位组装固相微萃取涂层与高效液相色谱联用测定多环芳烃

doi:10.11944/j.issn.1000-0518.2020.02.190235

摘要/Abstract

摘要：

利用恒电势法在钛丝表面原位阳极氧化组装固相微萃取(SPME)纤维,通过考察不同浓度电解质溶液和电解时间对二氧化钛纳米管(TiO₂NTs)形成及尺寸的影响来确定最佳的SPME纤维的形貌。结果表明,NH₄F在水相中的质量分数为0.5%,乙二醇在水相中的体积分数为50%,氧化电势为20 V,温度为25 ℃,氧化时间30 min的条件下,得到内径为100 nm,壁厚为25 nm的有序纳米管排列。利用组装得到的二氧化钛纳米管纤维涂层(TiO₂NTs/Ti)与高效液相色谱(HPLC)联用测定水样中的多环芳烃(PAHs)。在优化的萃取条件下,该方法灵敏度高,线性范围宽,选择性和重复性好,操作简便。利用此方法测量了实际水样中的PAHs浓度,得到了令人满意的分析结果。

关键词: 二氧化钛纳米管, 组装, 固相微萃取, 多环芳烃

Abstract:

In this article, solid phase microextraction (SPME) fibers were assembled by in situ anodization on the surface of titanium wire with a constant voltage and anodization time. Effect of the electrolyte solutions of different concentrations (concentration of NH₄F and ethylene glycol) and electrolysis time on the formation and size of TiO₂ nanotubes (TiO₂NTs) was investigated. TiO₂NTs arrays were arranged with the wall thickness of 25 nm and the pore diameter of 100 nm in ethylene glycol and water (volume ratio 1:1) containing 0.5% mass fraction of NH₄F at 20 V for 30 min at 25 ℃. Development of titanium dioxide nanotube array as a fiber coating for solid-phase microextraction coupled to high performance liquid chromatography for sensitive determination of polycyclic aromatic hydrocarbons (PAHs) in water. Under the optimized SPME conditions, this method has a higher sensitivity, wider linear range, better selectivity and repetition, and was easier to operate. The proposed method was successfully applied to the preconcentration and determination of target PAHs in river water and wastewater samples with satisfactory analytical results.

Key words: titanium dioxide nanotube, assemble, solid phase microextraction, polycyclic aromatic hydrocarbons

马明广, 魏云霞. 钛丝原位组装固相微萃取涂层与高效液相色谱联用测定多环芳烃[J]. 应用化学, 2020, 37(2): 218-226.

MA Mingguang, WEI Yunxia. Fabrication of Solid Phase Microextraction Fibers of Titanium Wires and Its Application[J]. Chinese Journal of Applied Chemistry, 2020, 37(2): 218-226.

参考文献

[1]	Gong D,Grimes C A,Varghese O K,et al.Titanium Oxide Nanotube Arrays Prepared by Anodic Oxidation[J]. J Mater Res,2001,16(12):3331-3334.
[2]	Sun M,Feng J J,Qiu H M,et al.CNT-TiO2 Coating Bonded onto Stainless Steel Wire as a Novel Solid-Phase Microextraction Fiber[J]. Talanta,2013,114(4):60-65.
[3]	García-Valverde M T,Lucena R,Cárdenas S,et al. Titanium-Dioxide Nanotubes as Sorbents in (micro)Extraction Techniques[J]. Trends Anal Chem,2014,62:37-45.
[4]	LI Zhen,LIU Hanmeng,YAO Zhixia,et al.Preparation and Characterization of Titanium Dioxide Nanotube Array/Titanium pH Electrode[J]. Chinese J Anal Chem,2018,46(12):120-126(in Chinese). 李振,刘寒蒙,姚志霞,等. 二氧化钛纳米管阵列/钛pH电极制备与表征[J]. 分析化学,2018,46(12):120-126.
[5]	Liu X,Liu Z Q,Lu J L,et al.Electrodeposition Preparation of Ag Nanoparticles Loaded TiO2 Nanotube Arrays with Enhanced Photocatalytic Performance[J]. Appl Surf Sci,2014,288(1):513-517.
[6]	MAO Yulu,ZHANG Xi,XU Mai,et al.Preparation of Ti/TiO2 Nanotube Arrays/PbO2-Pr Electrode and Its Application in Electrocatalytic Degradation of Organic Wastewater[J]. Chinese J Appl Chem,2018,35(5):582-588(in Chinese). 毛雨路,张西,徐迈,等. Ti/TiO2纳米管阵列/PbO2-Pr电极制备及在电氧化有机废水中应用[J]. 应用化学,2018,35(5):582-588.
[7]	Cabanas-Polo S,Boccaccini A R.Electrophoretic Deposition of Nanoscale TiO2:Technology and Applications[J]. J Eur Ceram Soc,2015,36(2):265-283.
[8]	Madichie C,Greenway G M,McCreedy T. The Effects of Surfactants on the Analysis of Organic Pollutants in Natural Waters[J]. Anal Chim Acta,1999,392(1):39-46.
[9]	Tsai P J,Shieh H Y,Lee W J,et al.Characterization of PAHs in the Atmosphere of Carbon Black Manufacturing Workplaces[J]. J Hazard Mater,2002,91(91):25-42.
[10]	Wenzl T,Simon R,Kleiner J,et al.Analytical Methods for Polycyclic Aromatic Hydrocarbons(PAHs) in Food and the Environment Needed for New Food Legislation in the European Union[J]. Trends Anal Chem,2006,25(7):716-725.
[11]	Riddle S G,Robert M A,Jakober C A,et al.Size Distribution of Trace Organic Species Emitted from Light-Duty Gasoline Vehicles[J]. Environ Sci Technol,2007,41(21):7464-7471.
[12]	Zencak Z,Klanova J,Holoubek I,et al.Source Apportionment of Atmospheric PAHs in the Western Balkans by Natural Abundance Radiocarbon Analysis[J]. Environ Sci Technol,2007,41(11):3850-3855.
[13]	Zhou Y Y,Yan X P,Kim K N,et al.Exploration of Coordination Polymer as Sorbent for flow Injection Solid-Phase Extraction On-line Coupled with High-Performance Liquid Chromatography for Determination of Polycyclic Aromatic Hydrocarbons in Environmental Materials[J]. J Chromatogr A,2006,1116(1):172-178.
[14]	Li K,Li H F,Liu L B,et al.Solid-Phase Extraction with C30 Bonded Silica for Analysis of Polycyclic Aromatic Hydrocarbons in Airborne Particulate Matters by Gas Chromatography-Mass Spectrometry[J]. J Chromatogr A,2007,1154(1/2):74-80.
[15]	García-Falcón M S,Pérez-Lamela M,Simal-Gándara J. Comparison of Strategies for Extraction of High Molecular Weight Polycyclic Aromatic Hydrocarbons from Drinking Waters[J]. J Agric Food Chem,2004,52(23):6897-6903.
[16]	Ishizaki A,Saito K,Hanioka N,et al.Determination of Polycyclic Aromatic Hydrocarbons in Food Samples by Automated On-line In-tube Solid-Phase Microextraction Coupled with High-Performance Liquid Chromatography-Fluorescence Detection[J]. J Chromatogr A,2010,1217(35):5555-5563.
[17]	Burkhardt M R,Zaugg S D,Burbank T L,et al.Pressurized Liquid Extraction Using Water/Isopropanol Coupled with Solid-Phase Extraction Clean up for Semivolatile Organic Compounds, Polycyclic Aromatic Hydrocarbons(PAH), and Alkylate PAH Homolog Groups in Sediment[J]. Anal Chim Acta,2005,549(1/2):104-116.
[18]	Hartonen K,Bøwadt S,Dybdahl H P,et al.Nordic Laboratory Intercomparison of Supercritical Fluid Extraction for the Determination of Total Petroleum Hydrocarbon, Polychlorinated Biphenyls and Polycyclic Aromatic Hydrocarbons in Soil[J]. J Chromatogr A,2002,958(1/2):239-248.
[19]	Macak J M,Hildebrand H,Marten-Jahns U,et al.Mechanistic Aspects and Growth of Large Diameter Self-organized TiO2 Nanotubes[J]. J Electroanal Chem,2008,621(2):254-266.
[20]	Macak J M,Gong B G,Hueppe M,et al.Filling of TiO2 Nanotubes by Self-doping and Electrodeposition[J]. Adv Mater,2007,19(19):3027-3031.
[21]	Valota A,LeClere D J,Skeldon P,et al. Influence of Water Content on Nanotubular Anodic Titania Formed in Fluoride/Glycerol Electrolytes[J]. Electrochim Acta,2009,54(15):4321-4327.
[22]	Boyd-Boland A A,Pawliszyn J B. Solid-Phase Microextraction of Nitrogen-Containing Herbicides[J]. J Chromatogr A,1995,704(1):163-172.