Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543, Singapore.
J Chromatogr A. 2013 Jan 25;1274:28-35. doi: 10.1016/j.chroma.2012.12.017. Epub 2012 Dec 19.
For the first time, a novel low-density solvent-based vortex-assisted surfactant-enhanced-emulsification liquid-liquid microextraction (LDS-VSLLME) was developed for the fast, simple and efficient determination of six phthalate esters (PEs) in bottled water samples followed by gas chromatography-mass spectrometry (GC-MS). In the extraction procedure, the aqueous sample solution was injected into a mixture of extraction solvent (toluene) and surfactant (cetyltrimethyl ammonium bromide), which were placed in a glass tube with conical bottom, to form an emulsion by the assistance of vortex agitation. After extraction and phase separation by centrifugation, and removal of the spent sample, the toluene extract was collected and analyzed by GC-MS. The addition of surfactant enhanced the dispersion of extraction solvent in aqueous sample and was also favorable for the mass transfer of the analytes from the aqueous sample to the extraction solvent. Moreover, using a relatively less toxic surfactant as the emulsifier agent overcame the disadvantages of traditional organic dispersive solvents that are usually highly toxic and expensive and might conceivably decrease extraction efficiency to some extent since they are not as effective as surfactants themselves in generating an emulsion. With the aid of surfactant and vortex agitation to achieve good organic extraction solvent dispersion, extraction equilibrium was achieved within 1 min, indicating it was a fast sample preparation technique. Another prominent feature of the method was the simple procedure to collect a less dense than water solvent by a microsyringe. After extraction and phase separation, the aqueous sample was removed using a 5-mL syringe, thus leaving behind the extract, which was retrieved easily. This novel method simplifies the use of low-density solvents in DLLME. Under the optimized conditions, the proposed method provided good linearity in the range of 0.05-25 μg/L, low limits of detection (8-25 ng/L) and good enrichment factors up to 290. The proposed method was successfully applied to the extraction of PEs in bottled water samples as a fast, efficient, and convenient method.
首次开发了一种新型的基于低相对密度溶剂的涡旋辅助表面活性剂强化乳化液液微萃取(LDS-VSLLME),用于快速、简单、高效地测定瓶装水样中的六种邻苯二甲酸酯(PEs),并结合气相色谱-质谱法(GC-MS)进行分析。在萃取过程中,将水样注入装有萃取溶剂(甲苯)和表面活性剂(十六烷基三甲基溴化铵)的玻璃管中,通过涡旋搅拌形成乳液。萃取和离心分层后,去除用过的样品,收集甲苯萃取液并进行 GC-MS 分析。表面活性剂的加入增强了萃取溶剂在水样中的分散性,有利于分析物从水样向萃取溶剂的传质。此外,使用相对毒性较小的表面活性剂作为乳化剂克服了传统有机分散溶剂的缺点,这些溶剂通常毒性大且昂贵,并且在一定程度上可能降低萃取效率,因为它们在生成乳液方面不如表面活性剂本身有效。在表面活性剂和涡旋搅拌的辅助下,实现了良好的有机萃取溶剂分散,萃取平衡在 1 分钟内达到,表明这是一种快速的样品制备技术。该方法的另一个突出特点是使用微量注射器简单地收集比水轻的溶剂。萃取和分层后,使用 5mL 注射器去除水样,从而留下易于回收的萃取液。这种新型方法简化了低密度溶剂在 DLLME 中的使用。在优化条件下,该方法在 0.05-25μg/L 范围内呈现良好的线性,检测限低(8-25ng/L),富集因子高达 290。该方法成功应用于瓶装水样中 PEs 的提取,是一种快速、高效、方便的方法。