Department of Chemistry, Tarbiat Modares University, Tehran, Iran.
Department of Chemistry, Tarbiat Modares University, Tehran, Iran.
J Chromatogr A. 2021 Jan 11;1636:461756. doi: 10.1016/j.chroma.2020.461756. Epub 2020 Dec 5.
A miscible-immiscible deep eutectic solvent (DES) containing monoethanolamine/4-methoxyphenol was used as an extraction solvent in a homogeneous liquid-liquid microextraction (HLLME). The method was used to preconcentrate chlorobenzenes in water samples followed by separating and analyzing them by gas chromatography-mass spectroscopy (GC-MS). A special feature of the new extraction method is that a green miscible solvent was used as an extractant in the HLLME method. The developed extraction technique provided enrichment factors in the range of 13.1-42.1 for extraction from only 1.0 mL of the aqueous sample solution. The effects of various experimental parameters were investigated and optimized. The optimal conditions were as follows: vortex time: 30.0 s, bubbling CO gas: 1.0 min, salt concentration: 5.0% w/v, rate and time of centrifuge: 4000.0 rpm and 3.0 min, respectively, and DES volume: 30.0 µL. The limit of detections and the limit of quantifications for the four targeted analytes varied from 0.01-0.15 and 0.025-0.5 µg L, respectively. The precision and long-term precision tests for the developed method were found to be less than 11.0%. Two real samples, including toilet air freshener and car perfume, were analyzed. The applied DES in the HLLME method provides a fast means of sample preparation for environmental aqueous sample solutions.
一种含有单乙醇胺/4-甲氧基苯酚的可混溶性-不混溶性深共晶溶剂 (DES) 被用作均相液-液微萃取 (HLLME) 中的萃取溶剂。该方法用于预浓缩水样中的氯苯,然后通过气相色谱-质谱联用仪 (GC-MS) 对其进行分离和分析。新萃取方法的一个特点是,在 HLLME 方法中使用了绿色可混溶性溶剂作为萃取剂。所开发的萃取技术仅从 1.0 mL 水样品溶液中提取时,提供了 13.1-42.1 的富集因子。研究并优化了各种实验参数的影响。最佳条件如下:涡旋时间:30.0 s,鼓泡 CO 气:1.0 min,盐浓度:5.0% w/v,离心速率和时间:4000.0 rpm 和 3.0 min,DES 体积:30.0 µL。四个目标分析物的检测限和定量限分别为 0.01-0.15 和 0.025-0.5 µg L。所开发方法的精密度和长期精密度测试发现小于 11.0%。分析了两个实际样品,包括厕所空气清新剂和汽车香水。HLLME 方法中应用的 DES 为环境水样的快速样品制备提供了一种手段。