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氧化单壁碳纳米角作为吸附剂用于多孔中空纤维直接浸入式固相微萃取水中三嗪类化合物的测定。

Oxidized single-walled carbon nanohorns as sorbent for porous hollow fiber direct immersion solid-phase microextraction for the determination of triazines in waters.

机构信息

Department of Analytical Chemistry, Institute of Fine Chemistry and Nanochemistry, University of Córdoba, Cordoba, Spain.

出版信息

Anal Bioanal Chem. 2013 Mar;405(8):2661-9. doi: 10.1007/s00216-013-6716-5. Epub 2013 Jan 31.

Abstract

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.

摘要

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。

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