期刊
TALANTA
卷 179, 期 -, 页码 775-783出版社
ELSEVIER SCIENCE BV
DOI: 10.1016/j.talanta.2017.12.012
关键词
Metal-organic frameworks; Dispersive miniaturized solid-phase extraction; Sample preparation; Pollutants; Environmental waters
资金
- Spanish Ministry of Economy and Competitiveness (MINECO) [MAT2014-57465-R]
- FPI [MAT2014-57465-R]
- Cabildo de Tenerife under the 'Agustin de Betancourt' Program
Five metal-organic frameworks (MOFs), specifically HKUST-1, MOF-5(Zn), MIL-53(Al), UiO-64 and MOF-74(Zn) are synthesized, characterized, and utilized in a miniaturized solid-phase extraction method under dispersive mode (D-mu SPE) for the determination of six pollutants of different nature, including one polycyclic aromatic hydrocarbon, two hormones, two drugs, and one disinfectant, from environmental waters (tap water and wastewater). A discussion of possible interactions justifying the partitioning of target analytes to the MOFs is included, considering not only the analytes' physicochemical characteristics but also those of MOFs: metal nature, structural environment of MOF pores, pore size and pore aperture widths, among others. MIL-53(Al) is selected for its versatility and high extraction efficiency for the target compounds. The D-pSPE method using MIL-53(Al) is optimized and used in combination with high-performance liquid chromatography (HPLC) with diode array detector (DAD) or liquid-chromatography with time-of-flight mass spectrometric detector (LC-TOF). Under optimum conditions, only 5 mg of MIL-53(Al) are required for 10 mL of water, with the aid of 5 min of vortex and 5 min of centrifugation. Elution is accomplished with 200 mu L of acetonitrile (3 times), and evaporation down to 100 mu L before LC injection. Detection limits down to 0.040 mu g L-1 for triclosan and 0.013 mu g L-1 for atrazine are obtained for the entire method using HPLC-DAD and LC-TOF, respectively. The method, operating at low spiked levels (2 mu g L-1 for HPLC-DAD and 0.7 mu g L-1 for LC-TOF), is also characterized for average relative recoveries of 109% and 105%; relative standard deviation values lower than 8.7% and 7.5%; and average extraction efficiencies of 41.2% and 49.1%; using HPLC-DAD and LC-TOF, respectively; while demonstrating adequate analytical performance with complex samples such as wastewaters.
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