Planas Carles, Palacios Oscar, Ventura Francesc, Rivera Josep, Caixach Josep
Mass Spectrometry Laboratory, Department of Ecotechnologies, IIQAB, CSIC, Jordi Girona Salgado 18, 08034 Barcelona, Spain.
Talanta. 2008 Aug 15;76(4):906-13. doi: 10.1016/j.talanta.2008.04.060. Epub 2008 May 8.
A method based on automated solid-phase extraction (SPE) and isotope dilution gas chromatography/high resolution mass spectrometry (GC/HRMS) has been developed for the analysis of nine nitrosamines in water samples. The combination of automated SPE and GC/HRMS for the analysis of nitrosamines has not been reported previously. The method shows as advantages the selectivity and sensitivity of GC/HRMS analysis and the high efficiency of automated SPE with coconut charcoal EPA 521 cartridges. Low method detection limits (MDLs) were achieved, along with a greater facility of the procedure and less dependence on the operator with regard to the methods based on manual SPE. Quality requirements for isotope dilution-based methods were accomplished for most analysed nitrosamines, regarding to trueness (80-120%), method precision (<15%) and MDLs (0.08-1.7 ng/L). Nineteen water samples (16 samples from a drinking water treatment plant {DWTP}, 2 chlorinated samples from a sewage treatment plant {STP} effluent, and 1 chlorinated sample from a reservoir) were analysed. Concentrations of nitrosamines in the STP effluent were 309.4 and 730.2 ng/L, being higher when higher doses of chlorine were applied. N-Nitrosodimethylamine (NDMA) and N-nitrosodiethylamine (NDEA) were the main compounds identified in the STP effluent, and NDEA was detected above 200 ng/L, regulatory level for NDMA in effluents stated in Ontario (Canada). Lower concentrations of nitrosamines were found in the reservoir (20.3 ng/L) and in the DWTP samples (n.d. -28.6 ng/L). NDMA and NDEA were respectively found in the reservoir and in treated and highly chlorinated DWTP samples at concentrations above 10 ng/L (guide value established in different countries). The highest concentrations of nitrosamines were found after chlorination and ozonation processes (ozonated, treated and highly chlorinated water) in DWTP samples.
已开发出一种基于自动固相萃取（SPE）和同位素稀释气相色谱/高分辨率质谱（GC/HRMS）的方法，用于分析水样中的九种亚硝胺。自动SPE和GC/HRMS相结合用于分析亚硝胺，此前尚未见报道。该方法具有GC/HRMS分析的选择性和灵敏度以及使用椰壳炭EPA 521柱的自动SPE的高效性等优点。实现了低方法检测限（MDL），并且与基于手动SPE的方法相比，该程序更简便，对操作人员的依赖性更小。对于大多数分析的亚硝胺，基于同位素稀释的方法在真实性（80-120%）、方法精密度（<15%）和MDL（0.08-1.7 ng/L）方面达到了质量要求。分析了19个水样（16个来自饮用水处理厂{DWTP}的样品、2个来自污水处理厂{STP}出水的氯化样品和1个来自水库的氯化样品）。STP出水中亚硝胺的浓度分别为309.4和730.2 ng/L，当使用更高剂量的氯时浓度更高。N-亚硝基二甲胺（NDMA）和N-亚硝基二乙胺（NDEA）是在STP出水中鉴定出的主要化合物，并且检测到NDEA高于200 ng/L，这是加拿大安大略省规定的废水中NDMA的监管水平。在水库（20.3 ng/L）和DWTP样品（未检出-28.6 ng/L）中发现亚硝胺的浓度较低。在水库以及经过处理和高度氯化的DWTP样品中分别发现NDMA和NDEA的浓度高于10 ng/L（不同国家确定的指导值）。在DWTP样品中，氯化和臭氧化过程（臭氧化、处理和高度氯化的水）后发现亚硝胺的浓度最高。
