Department of Analytical Chemistry, Institute of Fine Chemistry and Nanochemistry, University of Córdoba, Cordoba, Spain.
Anal Bioanal Chem. 2013 Mar;405(8):2661-9. doi: 10.1007/s00216-013-6716-5. Epub 2013 Jan 31.
This paper evaluates the potential of oxidized single-walled carbon nanohorns (o-SWNHs) immobilized on the pores of a hollow fiber (HF) for the direct immersion solid-phase microextraction of triazines from waters. The fabrication of the device requires the oxidation of the nanoparticles by means of microwave irradiation in order to obtain a homogeneous dispersion in methanol. Then, a porous hollow fiber is immersed in the methanolic dispersion of the o-SWNHs under ultrasound stirring. This procedure permits the immobilization of the o-SWNHs in the pores of the hollow fiber. For the extraction, a stainless steel wire was introduced inside the fiber to allow the vertical immersion of the o-SWNHs-HF in the aqueous standard/water sample. The triazines were preconcentrated on the immobilized o-SWNHs and further eluted using 150 μL of methanol. The solvent was evaporated and the residue reconstituted in 10 μL of methanol for sensitivity enhancement. Gas chromatography-mass spectrometry was selected as instrumental technique. The limits of detection were between 0.05 and 0.1 μg L(-1) with an excellent precision (expressed as relative standard deviation) between runs (below 10.2 %) and between fibers (below 12.8 %). Finally, the method was applied to the determination of the triazines in fortified waters, an average recovery value of 90 % being obtained.
本文评估了氧化单壁纳米碳管(o-SWNHs)固定在中空纤维(HF)孔中的潜力,用于直接浸入固相微萃取水中的三嗪。该装置的制备需要通过微波辐射氧化纳米颗粒,以获得甲醇中的均匀分散体。然后,将多孔中空纤维浸入 o-SWNHs 的甲醇分散体中,并在超声搅拌下进行。该程序允许 o-SWNHs 在中空纤维的孔中固定。对于萃取,将不锈钢丝引入纤维内部,以允许 o-SWNHs-HF 垂直浸入水标准/水样中。三嗪被固定在 o-SWNHs 上预浓缩,然后用 150μL 甲醇洗脱。将溶剂蒸发,并将残留物重新溶解在 10μL 甲醇中以增强灵敏度。选择气相色谱-质谱作为仪器技术。检出限在 0.05 至 0.1μg/L 之间,具有极好的精密度(以运行之间的相对标准偏差表示),低于 10.2%,纤维之间低于 12.8%。最后,该方法应用于加标水中三嗪的测定,获得了 90%的平均回收率。