Key Laboratory of Analytical Chemistry for Biology and Medicine, Ministry of Education, Department of Chemistry, Wuhan University, Wuhan 430072, China.
Key Laboratory of Analytical Chemistry for Biology and Medicine, Ministry of Education, Department of Chemistry, Wuhan University, Wuhan 430072, China.
J Chromatogr A. 2014 Aug 22;1356:45-53. doi: 10.1016/j.chroma.2014.06.062. Epub 2014 Jun 24.
In this work, metal-organic frameworks (MOFs, Al-MIL-53-NH₂) were synthesized via the hydrothermal method, and novel polydimethylsiloxane/metal-organic framework (PDMS/MOFs, PDMS/Al-MIL-53-NH₂)-coated stir bars were prepared by the sol-gel technique. The preparation reproducibility of the PDMS/MOFs-coated stir bar was good, with relative standard deviations (RSDs) ranging from 4.8% to 14.9% (n=7) within one batch and from 6.2% to 16.9% (n=6) among different batches. Based on this fact, a new method of PDMS/MOFs-coated stir bar sorptive extraction (SBSE) and ultrasonic-assisted liquid desorption (UALD) coupled with high performance liquid chromatography-fluorescence detection (HPLC-FLD) was developed for the determination of polycyclic aromatic hydrocarbons (PAHs) in environmental water samples. To obtain the best extraction performance for PAHs, several parameters affecting SBSE, such as extraction time, stirring rate, and extraction temperature, were investigated. Under optimal experimental conditions, wide linear ranges and good RSDs (n=7) were obtained. With enrichment factors (EFs) of 16.1- to 88.9-fold (theoretical EF, 142-fold), the limits of detection (LODs, S/N=3) of the developed method for the target PAHs were found to be in the range of 0.05-2.94 ng/L. The developed method was successfully applied to the analysis of PAHs in Yangtze River and East Lake water samples.
在这项工作中,通过水热法合成了金属有机骨架(MOFs,Al-MIL-53-NH₂),并通过溶胶-凝胶技术制备了新型聚二甲基硅氧烷/金属有机骨架(PDMS/MOFs,PDMS/Al-MIL-53-NH₂)-涂层搅拌棒。PDMS/MOFs 涂层搅拌棒的制备重现性良好,同一批次内的相对标准偏差(RSD)范围为 4.8%至 14.9%(n=7),不同批次之间的 RSD 范围为 6.2%至 16.9%(n=6)。基于这一事实,开发了一种新的聚二甲基硅氧烷/金属有机骨架(PDMS/MOFs)涂层搅拌棒吸附萃取(SBSE)和超声辅助液解吸(UALD)与高效液相色谱-荧光检测(HPLC-FLD)相结合的方法,用于测定环境水样中的多环芳烃(PAHs)。为了获得对 PAHs 的最佳萃取性能,研究了影响 SBSE 的几个参数,如萃取时间、搅拌速率和萃取温度。在最佳实验条件下,获得了较宽的线性范围和良好的 RSD(n=7)。通过富集因子(EF)为 16.1 至 88.9 倍(理论 EF,142 倍),该方法对目标 PAHs 的检测限(LOD,S/N=3)范围为 0.05 至 2.94ng/L。该方法成功应用于长江和东湖水样中 PAHs 的分析。