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目的建立优化固相萃取-气相色谱质谱(SPE-GC-MS)同时检测饮用水中9种亚硝胺类物质方法条件。方法通过固相萃取前处理以及优化后的气相色谱质谱法对样品净化浓缩,同时通过样品回收率、精密度、方法检出限(MDL)、测定下限、标准曲线对建立的方法进行验证。结果 9种亚硝胺的保留时间在9.819~20.541min,在10~1000μg/L均线性范围良好(R~2>0.999),MDL在2.27~6.20ng/L,低浓度(50ng/L)加标回收率为62.32%~89.71%,中(100 ng/L)、高浓度(200 ng/L)加标回收率为73.43%~109.66%,相对标准偏差(RSD)均<10,自来水加标回收率为74.62%~102.74%。结论建立的SPE-GC-MS法满足检测饮用水中9种亚硝胺类物质的要求。
Objective To establish a method for the simultaneous determination of nine nitrosamines in drinking water by gas chromatography-mass spectrometry (SPE-GC-MS). Methods The sample was purified and concentrated by pre-SPE and gas chromatography-mass spectrometry (GC-MS), and the established method was validated by the sample recovery, precision, method detection limit (MDL), determination of lower limit and standard curve. Results The retention times of 9 kinds of nitrosamines ranged from 9.819 to 20.541 min. The average linear range was from 10 to 1000 μg / L (R ~ 2> 0.999), the MDL was 2.27 ~ 6.20 ng / L and the low concentration (50 ng / L) The standard recoveries were between 62.32% and 89.71%, with the recoveries of 100 ng / L and 200 ng / L were 73.43% -109.66%, and the relative standard deviations (RSDs) were all less than 10 The recoveries ranged from 74.62% to 102.74%. Conclusion The established SPE-GC-MS met the requirements of detecting nine nitrosamines in drinking water.