School of Environment, Tsinghua University, No. 30 Shuangqing Road, Hai Dian District, Beijing 100084, China.
SHANGHAI Soong Ching Ling School, Shanghai 200000, China.
Int J Environ Res Public Health. 2022 Dec 12;19(24):16680. doi: 10.3390/ijerph192416680.
The ability to effectively detect N-nitrosamine compounds by liquid chromatography-tandem mass spectrometry presents a challenge due to the problems of high detection limits and difficulty in simultaneous N-nitrosamine compound detection. In order to overcome these limitations, this study reduced the detection limit of N-nitrosamine compounds by applying n-hexane pre-treatment to remove non-polar impurities before the conventional process of column extraction. In addition, ammonium acetate was used as the mobile phase to enhance the retention of nitrosamine target substances on the chromatographic column, with formic acid added to the mobile phase to improve the ionization level of N-nitrosodiphenylamine, to achieve the simultaneous detection of multiple N-nitrosamine compounds. Applying these modifications to the established detection method allowed the rapid and accurate detection of N-nitrosamine in water within 12 min. The linear relationship, detection limit, quantification limit and sample spiked recovery rate of nine types of nitrosamine compound were investigated, showing that the correlation coefficient ranged from 0.9985-0.9999, while the detection limits of the instrument and the method were 0.280-0.928 µg·L and 1.12-3.71 ng·L, respectively. The spiked sample recovery rate ranged from 64.2-83.0%, with a standard deviation of 2.07-8.52%, meeting the requirements for trace analysis. The method was applied to the detection of N-nitrosamine compounds in nine groundwater samples in Wuhan, China, and showed that the concentrations of N-nitrosodimethylamine and NDEA were relatively high, highlighting the need to monitor water bodies with very low levels of pollutants and identify those requiring treatment.
采用正己烷预处理,在常规柱萃取前去除非极性杂质,降低了检测限,同时应用乙酸铵作为流动相增强了色谱柱上的亚硝胺目标物的保留,在流动相中添加甲酸以提高 N-亚硝基二苯胺的离子化水平,从而实现多种 N-亚硝胺化合物的同时检测。将这些改进应用于已建立的检测方法中,可在 12 min 内快速准确地检测水中的 N-亚硝胺。考察了九种亚硝胺化合物的线性关系、检测限、定量限和样品加标回收率,结果表明,相关系数在 0.9985-0.9999 之间,仪器和方法的检测限分别为 0.280-0.928 µg·L 和 1.12-3.71 ng·L。加标样品的回收率在 64.2-83.0%之间,标准偏差为 2.07-8.52%,满足痕量分析的要求。该方法应用于检测中国武汉的九种地下水样品中的 N-亚硝胺化合物,结果表明 N-二甲基亚硝胺和 NDEA 的浓度相对较高,这突出表明需要监测污染物水平非常低的水体,并识别需要处理的水体。