饮用水中9种痕量亚硝胺类化合物的分析方法研究

Analytical methodology of 9 trace nitrosamine compounds in drinking water

建立了9种亚硝胺类化合物(NDMA,NMEA,NDEA,NDPA,NDBA,NPiP,NPyr, NMor, NDphA)的SPE-UPLC-MS检测方法。优化了流动相、离子源、萃取柱、样品保存条件、样品保存时间5个条件,实验结果表明:流动相使用0.1%(V/V)的甲酸水和甲醇,仪器响应最好;活性炭萃取柱萃取除NDPhA的8种物质,使用大气压电离源(APCI)测定;HLB萃取柱萃取NDphA,使用电喷雾电离源(ESI)测定;样品使用硫代硫酸钠进行脱氯保存;样品在7 d之内进行测定。对纯水、地表水、出厂水中的9种亚硝胺化合物进行加标测定,回收率范围为72.0%~128.9%,精密度范围为0.7%~20%。

An ultra high performance liquid chromatography/tandem mass spectrometry(UPLC-MS/MS) method for determination of 9 kinds of nitrosamine compounds(NDMA, NMEA, NDEA, NDPA, NDBA, NPiP, NPyr, NMor, NDphA) was developed. The conditions of mobile phase, ion source, extraction column, sample storage conditions and time were optimized. The optimum conditions were as following. The mobile phase was water mixed with 0.1%(V/V) formic acid and methanol. 8 substances were extracted by activated carbon extraction column and determined by atmospheric pressure ionization source(APCI) while NDphA was extracted by HLB extraction column and measured by electrospray ionization source(ESI). Samples were stored with sodium thiosulfate for dechlorination and should be measured within 7 days. The spiked determination of 9 nitrosamine compounds in pure water, surface water and treated water had an accuracy range of 72.0%-128.9% and a precision range of 0.7%-20%.