Kodamatani Hitoshi, Yamazaki Shigeo, Saito Keiitsu, Amponsaa-Karikari Abena, Kishikawa Naoya, Kuroda Naotaka, Tomiyasu Takashi, Komatsu Yu
Faculty of Science, Kagoshima University, 1-21-35 Korimoto, Kagoshima 890-0065, Japan.
J Chromatogr A. 2009 Jan 2;1216(1):92-8. doi: 10.1016/j.chroma.2008.11.025. Epub 2008 Nov 18.
A new method for the measurement of N-nitrosamines in part-per-trillion concentrations from water samples without preconcentration steps has been developed. This method is based on online UV irradiation after high-performance liquid chromatographic separation and subsequent luminol chemiluminescence detection without addition of an oxidant. It was confirmed that N-nitrosamines in basic aqueous solution were transformed to peroxynitrite by UV irradiation. The detection limits for this method were 1.5 ng/L, 2.9 ng/L, 3.0 ng/L, and 2.7 ng/L for N-nitrosodimethylamine, N-nitrosomorpholine, N-nitrosomethylethylamine, and N-nitrosopyrrolidine, respectively, at a signal-to-noise ratio of 3. The calibration graphs were linear in the range of 5-1000 ng/L for these N-nitrosamines. This method was used for the determination of N-nitrosamines in tap water, river water, and industrial plant effluent samples. The recoveries of N-nitrosodimethylamine, N-nitrosomorpholine, N-nitrosomethylethylamine, and N-nitrosopyrrolidine present in tap water sample at a concentration of 10 ng/L (mean+/-standard deviation, n=4) were (94.8+/-2.7)%, (102.0+/-6.9)%, (99.3+/-3.9)%, and (102.8+/-2.5)%, respectively. These results indicate that our proposed method can be applied satisfactorily to the determination of N-nitrosamines in water samples.
已开发出一种无需预浓缩步骤即可测定水样中万亿分之一浓度的N-亚硝胺的新方法。该方法基于高效液相色谱分离后的在线紫外线照射以及随后的鲁米诺化学发光检测,无需添加氧化剂。经证实,碱性水溶液中的N-亚硝胺通过紫外线照射可转化为过氧亚硝酸盐。该方法对N-二甲基亚硝胺、N-亚硝基吗啉、N-甲基乙基亚硝胺和N-亚硝基吡咯烷的检测限分别为1.5 ng/L、2.9 ng/L、3.0 ng/L和2.7 ng/L(信噪比为3)。这些N-亚硝胺的校准曲线在5-1000 ng/L范围内呈线性。该方法用于测定自来水、河水和工业废水样品中的N-亚硝胺。浓度为10 ng/L的自来水样品(平均值±标准偏差,n = 4)中N-二甲基亚硝胺、N-亚硝基吗啉、N-甲基乙基亚硝胺和N-亚硝基吡咯烷的回收率分别为(94.8±2.7)%、(102.0±6.9)%、(99.3±3.9)%和(102.8±2.5)%。这些结果表明,我们提出的方法可令人满意地应用于水样中N-亚硝胺的测定。