Department of Analytical Chemistry, Campus of Rabanales, University of Córdoba, Córdoba, Spain.
J Sep Sci. 2010 Mar;33(4-5):610-6. doi: 10.1002/jssc.200900679.
N-Nitrosamines (NAms) are suspected human carcinogens that have been identified as drinking water and wastewater pollutants. In this work, a sensitive screening/confirmation method was proposed for the determination of the most toxic NAms that can be found in water samples (N-nitrosodimethylamine, N-nitrosodiethylamine, N-nitrosodibutylamine, N-nitrosomorpholine, N-nitrosopiperidine, and N-nitrosopyrrolidine). A sample volume of 250 mL was first preconcentrated in an automatic SPE unit and then the extract was concentrated to a final volume of 10 microL (providing a preconcentration factor of 25,000). Aliquots of the extract were subjected to a rapid screening process (1.6 min) by using a short capillary polar column (1.5 m length) and GC with nitrogen-phosphorous detection. In this way, the high number of samples to be tested routinely in a water laboratory is simplified due to a reduction in the analysis time. Thus, the screening method acts as a filter that indicates whether target analytes are present, above or below the cut-off level (3.8 or 10.4 ng/L), giving no false negatives at concentrations below the guide values for NAms in drinking water established by different countries. Positive samples (tap and swimming pool waters) were then confirmed by GC-MS detection.
亚硝胺(NAs)被怀疑是人类致癌物,已被确定为饮用水和废水污染物。在这项工作中,提出了一种灵敏的筛选/确证方法,用于测定水样中存在的最有毒的 NAs(二甲基亚硝胺、二乙基亚硝胺、二正丁基亚硝胺、吗啉基亚硝胺、哌啶基亚硝胺和吡咯烷基亚硝胺)。首先将 250 mL 样品体积在自动 SPE 单元中预浓缩,然后将提取物浓缩至最终体积 10 μL(提供 25,000 倍的浓缩因子)。提取液的等分试样通过使用短毛细管极性柱(1.5 m 长度)和氮磷检测的 GC 进行快速筛选过程(1.6 分钟)。通过这种方式,由于分析时间的减少,简化了水实验室中常规测试的大量样品。因此,筛选方法充当指示是否存在目标分析物的过滤器,高于或低于截止水平(3.8 或 10.4 ng/L),在低于不同国家为饮用水中 NAs 设定的指导值的浓度下不会出现假阴性。然后通过 GC-MS 检测对阳性样品(自来水和游泳池水)进行确证。