地下水中102种酸性、碱性和中性有机污染物的气相色谱-质谱法同时快速测定

Simultaneous and Rapid Determination of 102 Acidic,Alkaline and Neutral Organic Pollutants in Groundwater by Gas Chromatography-Mass Spectrometry

建立了同时快速检测地下水中102种酸性、碱性和中性有机污染物的气相色谱-质谱(GC-MS)分析方法,所建方法涉及苯酚、苯胺、苯基醚、多氯萘、联苯等10类污染物。考察了酸性、碱性和中性有机污染物的同时提取条件,结果显示采用先中性、再酸性、后碱性三步液液萃取方式可以改善污染物的提取回收率,提高分析准确度和精密度。在优化条件下,除五氯苯酚外,101种目标物在各自的质量浓度范围内呈良好线性关系,相关系数(r)为0.995 0~0.999 9。地下水样品在低、中、高3个浓度水平的加标回收率分别为47.2%~126%、43.0%~117%、38.8%~120%,相对标准偏差(RSD,n=7)分别为1.1%~27%、2.6%~33%、2.9%~30%,方法检出限为1.8~19.7 ng/L(五氯苯酚、邻苯二甲酸二异丁酯、邻苯二甲酸二丁酯、邻苯二甲酸二(2-乙基)己酯除外)。方法应用于山西、河南等部分典型污染场地的地下水样品筛查,检出苯酚、苯胺、多环芳烃及其衍生物等24种酸、碱和中性有机污染物,点位检出率达到46.7%,水质明显呈点源污染特征。该方法灵敏、准确、简单、快速,可实现多目标物同时检测,有助于地下水中有机污染物快速筛查。

A gas chromatography-mass spectrometric(GC-MS)method was developed for simultaneous and rapid determination of 102 kinds of acidic, alkaline and neutral organic pollutants in groundwater,including phenol,aniline,phenyl ether,polychlorinated naphthalene and biphenyl,etc.The simultaneous extraction condition for 102 kinds of acidic,alkaline and neutral organic pollutants in groundwater was optimized. It was confirmed that three-step liquid-liquid extraction method(first in neutral,then in acidic,finally in alkaline condition)could improve the method’s extraction recoveries,accuracy and precision. Under the optimized conditions,the linear ranges of 101 targets except pentachlorophenol were obtained within there respective mass concentration ranges,with correlation coefficients(r)of 0. 995 0-0. 999 9. The limits of detection were in the range of 1. 8-19. 7 ng/L. The spiked recoveries for groundwater samples at low,medium and high concentration levels ranged from 47. 2%to 126%,43. 0%to 117%and 38. 8%to 120%,with the relative standard deviations(RSD, n = 7)of 1. 1%-27%,2. 6%-33%and 2. 9%-30%,respectively(expect for pentachlorophenol,diisobutyl phthalate,dibutyl phthalate and bis(2-ethylhexyl)phthalate).This method was used for the typical investigation on groundwater organic contamination in Shanxi and Henan. 24 pollutants were detected, such as phenol, aniline, polycyclic aromatic hydrocarbons and their derivatives.The point detection rate reached 46. 7%,which means the water quality presented the characteristics of point source pollution.The method is sensitive,accurate,simple and rapid,which will play an active role in the rapid screening of organic pollutants in groundwater in the future.