Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543, Singapore.
J Chromatogr A. 2011 Aug 5;1218(31):5040-6. doi: 10.1016/j.chroma.2011.05.069. Epub 2011 May 27.
For the first time, the low-density solvent-based solvent demulsification dispersive liquid-liquid microextraction was developed for the fast, simple, and efficient determination of 16 priority polycyclic aromatic hydrocarbons (PAHs) in environmental samples followed by gas chromatography-mass spectrometric (GC-MS) analysis. In the extraction procedure, a mixture of extraction solvent (n-hexane) and dispersive solvent (acetone) was injected into the aqueous sample solution to form an emulsion. A demulsification solvent was then injected into the aqueous solution to break up the emulsion, which turned clear and was separated into two layers. The upper layer (n-hexane) was collected and analyzed by GC-MS. No centrifugation was required in this procedure. Significantly, the extraction needed only 2-3 min, faster than conventional DLLME or similar techniques. Another feature of the procedure was the use of a flexible and disposable polyethylene pipette as the extraction device, which permitted a solvent with a density lighter than water to be used as extraction solvent. This novel method expands the applicability of DLLME to a wider range of solvents. Furthermore, the method was simple and easy to use, and some additional steps usually required in conventional DLLME or similar techniques, such as the aforementioned centrifugation, ultrasonication or agitation of the sample solution, or refrigeration of the extraction solvent were not necessary. Important parameters affecting the extraction efficiency were investigated in detail. Under the optimized conditions, the proposed method provided a good linearity in the range of 0.05-50 μg/L, low limits of detection (3.7-39.1 ng/L), and good repeatability of the extractions (RSDs below 11%, n=5). The proposed method was successfully applied to the extraction of PAHs in rainwater samples, and was demonstrated to be fast, efficient, and convenient.
首次发展了基于低黏度有机溶剂的溶剂分散液液微萃取,用于快速、简便、高效地测定环境样品中的 16 种优先多环芳烃(PAHs),随后采用气相色谱-质谱法(GC-MS)进行分析。在萃取过程中,将萃取溶剂(正己烷)和分散溶剂(丙酮)的混合物注入水样中,形成乳状液。然后将破乳溶剂注入水相中,破坏乳状液,使其变澄清并分成两相。上层(正己烷)被收集并通过 GC-MS 进行分析。此过程无需离心。重要的是,萃取仅需 2-3 分钟,比传统的 DLLME 或类似技术更快。该方法的另一个特点是使用灵活且一次性的聚乙烯移液管作为萃取装置,允许使用密度小于水的溶剂作为萃取溶剂。这种新方法将 DLLME 的适用性扩展到更广泛的溶剂范围。此外,该方法简单易用,无需常规 DLLME 或类似技术中通常需要的其他步骤,如上述的样品溶液离心、超声或搅拌,或萃取溶剂的冷藏。详细研究了影响萃取效率的重要参数。在优化条件下,该方法在 0.05-50 μg/L 范围内具有良好的线性,检出限低(3.7-39.1 ng/L),萃取重复性好(RSDs 低于 11%,n=5)。该方法成功应用于雨水样品中 PAHs 的提取,证明其快速、高效、方便。