Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543, Singapore.
J Chromatogr A. 2012 Nov 9;1263:1-6. doi: 10.1016/j.chroma.2012.09.016. Epub 2012 Sep 11.
Mixed zeolitic imidazolate framework 8 (ZIF-8) (nanometer and micron-sized) material were synthesized and applied as sorbent to sonication-assisted emulsification microextraction coupled to vortex-assisted porous membrane-protected micro-solid-phase extraction (SAE-VA-μ-SPE) of polycyclic aromatic hydrocarbons (PAHs) from water samples. Better extraction results was obtained by using the mixed sorbent for the extraction of PAHs from aqueous samples, than either nanometer or micron-sized ZIF-8 separately. The developed method proved to be a time-saving, highly efficient (total extraction procedure was less than 10 min), accurate and robust method for water sample pretreatment. Parameters influencing the extraction efficiency such as desorption solvent, extraction solvent volume, emulsification time, desorption time and salt concentration were investigated and optimized. The limits of detection from gas chromatography-mass spectrometric analysis of six PAHs after SAE-VA-μ-SPE ranged between 0.004 and 0.011 ng/ml. The linear ranges were from 0.05 to 50 ng/ml, and the correlation coefficient was higher than 0.9943. The proposed method provides an interesting and innovative approach of combining different microscale sample preparation methods to solve analytical problems that are not easily addressed by the individual procedure alone.
混合沸石咪唑酯骨架 8(ZIF-8)(纳米和微米级)材料被合成并用作吸附剂,用于声辅助乳化微萃取结合涡旋辅助多孔膜保护微固相萃取(SAE-VA-μ-SPE)从水样中萃取多环芳烃(PAHs)。与单独使用纳米或微米级 ZIF-8 相比,混合吸附剂更有利于从水样中萃取 PAHs。与单独使用纳米或微米级 ZIF-8 相比,该方法对于水样的预处理是一种省时、高效(总萃取过程不到 10 分钟)、准确和稳健的方法。考察并优化了影响萃取效率的参数,如解吸溶剂、萃取溶剂体积、乳化时间、解吸时间和盐浓度。通过 SAE-VA-μ-SPE 对 6 种 PAHs 的气相色谱-质谱分析,检测限在 0.004 至 0.011ng/ml 之间。线性范围为 0.05 至 50ng/ml,相关系数高于 0.9943。该方法提供了一种有趣且创新的方法,结合了不同的微尺度样品制备方法,以解决仅通过单个程序难以解决的分析问题。