摘要
建立了一种适合于测定地表水制自来水过程中痕量二甲基亚硝胺(Nitrosodimethylamine,NDMA)的固相萃取-高效液相色谱(High Performance Liquid Chromatorgragh,HPLC)分析方法。将样品溶液先经固相吸附萃取,再用甲醇洗脱,然后经氮吹浓缩,最后以体积比5/95的甲醇/水溶液为流动相,用高效液相色谱分离后于紫外波长228nm处检测,采用外标法定量分析。结果表明,NDMA在20~200μg/L范围内具有良好的线性,其R2大于0.9991,对60μg/L的加标回收率为101.60%,相对标准偏差(Relative Standard Deviation,RSD)为1.28%。获得各阶段操作精密度,在氮吹浓缩阶段,对50μg/L样品测试的RSD范围为0.22%~1.83%;在固相萃取阶段,对50ng/L水样浓缩后测试的RSD范围为0.24%~2.13%。由此,初步建立一种快速简单测定水体中20~200ng/L浓度范围的NDMA分析方法,为后续该方法的深化拓展,应用于其他水体中NDMA的分析方法研究奠定了基础。
A method of solid phase extraction-high performance liquid chromatography(HPLC)was established for the determination of trace NDMA during the preparation process of tap water using surface water.The sample solution was first extracted by solid phase adsorption,then eluted with methanol,then concentrated by nitrogen blowing,and finally the methanol/aqueous solution with a volume ratio of 5/95 as the mobile phase,separated by high performance liquid chromatography and detected at the UV wavelength of 228 nm,quantitative analysis was performed by using the external standard method.The results showed that NDMA had good linearity(R^(2)>0.9991)in the concentration range of 20μg/L to 200μg/L.The recovery was 101.60%and relative standard deviation(RSD)was 1.28%at the concentration of 60μg/L.For the operational precision at each stage:the RSD tested for the 50μg/L samples ranged from 0.22%to 1.83%in the nitrogen-blowing concentration,and the RSD tested after concentrating the 50 ng/L water samples ranged from 0.24%to 2.13%in the solid-phase extraction.A rapid and simple analysis method for the determination of NDMA in the range of 20 ng/L to 200 ng/L was preliminarily established,which laid a foundation for the further development of this method and the application of NDMA analysis methods in other water bodies.
作者
谢燕
田田
Olubunmi M.Olukowi
李新杰
张跃军
Xie Yan;Tian Tian;Olubunmi M.Olukowi;Li Xinjie;Zhang Yuejun(School of Chemistry and Chemical Engineering,Nanjing University of Science and Technology,Jiangsu,210094)
出处
《当代化工研究》
2023年第9期63-65,共3页
Modern Chemical Research
基金
2013年国家科技部“微污染原水强化混凝过程亚硝基二甲胺的形成规律与机理”(项目编号:21377054)。
关键词
NDMA
氮消毒副产物
原水
固相萃取
高效液相色谱
定量分析
NDMA
nitrogen disinfection byproduct
raw water
solid phase extraction
high performance liquid chromatography
quantitative analysis
