Departamento de Química Analítica, Facultad de Química, Universitat de València, 46100 Burjassot, Valencia, Spain.
Talanta. 2011 Sep 30;85(4):1990-5. doi: 10.1016/j.talanta.2011.07.048. Epub 2011 Jul 19.
A new, simple, fast and high sensitive analytical method based on dispersive liquid-liquid microextraction (DLLME) followed by gas chromatography-mass spectrometry (GC-MS) for the simultaneous determination of nitro musks in surface water and wastewater samples is presented. Different parameters, such as the nature and volume of both the extraction and disperser solvents and the ionic strength and pH of the aqueous donor phase, were optimized. Under the selected conditions (injection of a mixture of 1 mL of acetone as disperser solvent and 50 μL of chloroform as extraction solvent, no salt addition and no pH adjustment) the figures of merit of the proposed DLLME-GC-MS method were evaluated. High enrichment factors, ranging between 230 and 314 depending on the target analyte, were achieved, which redound to limits of detection in the ng L(-1) range (i.e., 4-33 ng L(-1)). The relative standard deviation (RSD) was below 5% for all the target analytes. Finally, the recoveries obtained for different water samples of diverse origin (sea, river, irrigation channel and water treatment plant) ranged between 87 and 116%, thus showing no matrix effects.
提出了一种新的、简单、快速和高灵敏度的分析方法,基于分散液液微萃取(DLLME),随后是气相色谱-质谱(GC-MS),用于同时测定地表水和废水中的硝基麝香。优化了不同的参数,如萃取和分散溶剂的性质和体积,以及水相供体的离子强度和 pH 值。在选定的条件下(注入 1 毫升丙酮作为分散溶剂和 50 μL 氯仿作为萃取溶剂,不添加盐,不调节 pH 值),评估了所提出的 DLLME-GC-MS 方法的优点。根据目标分析物的不同,获得了 230 到 314 之间的高富集因子,相当于 ng L(-1) 范围内的检出限(即 4-33 ng L(-1))。对于所有目标分析物,相对标准偏差(RSD)均低于 5%。最后,对于不同来源的不同水样(海水、河流、灌溉渠道和水处理厂),回收率在 87%到 116%之间,因此没有基质效应。