Farajzadeh Mir Ali, Ebrahimi Sadaf, Mehri Sina Mohammad, Afshar Mogaddam Mohammad Reza
Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz, Iran.
Engineering Faculty, Near East University, Mersin 10, Nicosia, 99138, North Cyprus, Turkey.
Sci Rep. 2025 May 31;15(1):19142. doi: 10.1038/s41598-025-04155-5.
Vortex-assisted liquid-liquid microextraction was used to extract and derivatize propylamine, butylamine, pentylamine, benzylamine, and sec-butylamine in various environmental water and refinery effluent samples. Herein, µL-volume of butyl chloroformate as a derivatization agent was added to 1,1,2-trichloroethane as an extraction solvent, allowing for simultaneous extraction and derivatization of the amines. The derivatization agent reacted with the amines in an alkaline medium under mild conditions to create their related carbamates. The carbamate derivatives obtained from primary amines performed well in gas chromatography system. Various affecting parameters of the method, such as the derivatization agent amount, type of extraction solvent, ionic strength of solution, pH, vortexing time, and centrifuging time and rate were carefully optimized. In the end, gas chromatography-flame ionization detector was used to separate, identify, and quantify the enriched derivatives. Under optimal conditions, enrichment factors varied from 440 to 515, while extraction recovery of the desired amines was between 88 and 103%. The limits of detection for amines ranged from 0.4 to 1.0 µg L, and inter- and intra-day precision were in the ranges of 2.2-5.8 and 1.0-3.3%, respectively. Also, relative recoveries were between 85 and 107%. This method proved to be valuable due to its simplicity, sensitivity, high precision, lack of need for special equipment, and high ability in the extraction and derivatization of the selected amines. The use of µL-volume of organic solvents made it economical and environmentally friendly.
采用涡旋辅助液液微萃取法对各类环境水样和炼油厂废水样品中的丙胺、丁胺、戊胺、苄胺和仲丁胺进行萃取和衍生化处理。在此，将微升体积的氯甲酸丁酯作为衍生化试剂加入到作为萃取溶剂的1,1,2 - 三氯乙烷中，实现胺类的同时萃取和衍生化。衍生化试剂在温和条件下于碱性介质中与胺类反应，生成其相应的氨基甲酸酯。从伯胺得到的氨基甲酸酯衍生物在气相色谱系统中表现良好。对该方法的各种影响参数，如衍生化试剂量、萃取溶剂类型、溶液离子强度、pH值、涡旋时间、离心时间和速率等进行了仔细优化。最后，使用气相色谱 - 火焰离子化检测器对富集后的衍生物进行分离、鉴定和定量。在最佳条件下，富集因子在440至515之间，而目标胺类的萃取回收率在88%至103%之间。胺类的检测限在0.4至1.0 μg/L范围内，日间和日内精密度分别在2.2 - 5.8%和1.0 - 3.3%范围内。此外，相对回收率在85%至107%之间。该方法因其简单、灵敏、高精度、无需特殊设备以及对所选胺类的萃取和衍生化能力强而被证明具有价值。使用微升体积的有机溶剂使其经济且环保。
