Abstract
A novel titanium dioxide nanotube (TiO2NTS) coated fiber for solid-phase microextraction (SPME) was prepared by in situ anodization of titanium wire in electrolyte containing ethylene glycol and ammonium fluoride (NH4F). The effects of different electrolyte solutions (NH4F and ethylene glycol) and oxidation voltages on the formation and size of TiO2NTs was studied. It was obtained from the experiment that TiO2NTs arrays were arranged with a wall thickness of 25 nm and the diameter of 100 nm pores in ethylene glycol and water (v/v, 1:1) containing NH4F of 0.5% (w/v) with a voltage of 20 V at 25 °C for 30 min. The TiO2NTs were used as solid-phase microextraction fiber coatings coupled with high-performance liquid chromatography (HPLC) in sensitive determination of polycyclic aromatic hydrocarbons (PAHs) in spiked real samples water. Under the optimized SPME conditions, the calibration curve has good linearity in the range of 0.20–500 μg·L−1, and the correlation coefficient (R2) is between 0.9980 and 0.9991. Relative standard deviations (RSDs) of 3.5–4.7% (n = 5) for single fiber repeatability and of 5.2% to 7.9% for fiber-to-fiber reproducibility (n = 3) was obtained. The limits of detection (LOD) (S/N = 3) and limits of quantification (LOQ) (S/N = 10) of PAHs were 0.03–0.05 µg·L−1 and 0.12–0.18 µg·L−1. The developed method was applied to the preconcentration and determination of trace PAHs in spiked real samples of water with good recoveries from 78.6% to 119% and RSDs from 4.3 to 8.9%, respectively.
Highlights
Solid-phase microextraction (SPME) has attracted extensive attention due to its high sensitivity, rapidity, simplicity and being free of solvents [1,2]
We investigated the effects of fluoride concentration and the amount of ethylene glycol on the formation and dimensions of the TiO2 NTs
Scanning electron microscope micrographs of TiO2 fibers were obtained on a field emission scanning electron microscope (Zeiss, Oberkochen, Germany) equipped with an energy dispersive X-ray (EDX) spectrometer
Summary
Solid-phase microextraction (SPME) has attracted extensive attention due to its high sensitivity, rapidity, simplicity and being free of solvents [1,2]. To overcome the above problems, an important development in the SPME fiber preparation technology is to obtain a coating with high mechanical strength and good chemical stability by using a metal as a matrix to improve the sensitivity and selectivity of the coating to the target compound [5,6,7,8,9]. In particular, have attracted the attention of many researchers due to their unique physical chemistry properties, including a large specific surface area, good chemical and thermal stability, and favorable adsorption performance [10,11] These metal fibers with high mechanical strength and nanostructured coatings exhibit higher extraction capacity, faster extraction rate and better extraction selectivity for the target analytes. Under the optimized SPME conditions, the fiber was used to measure PAHs in spiked real samples and from which we draw a satisfactory result
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