固相萃取-气相色谱质谱法同时测定地下水中苯胺、阿特拉津、3,3’—二氯联苯胺的方法研究

Simultaneous Determination of Aniline,Atrazine and 3,3'-Dichlorobenzidine in Groundwater by Solid Phase Extraction and Gas Chromatography-Mass Spectrometry

随着绿色发展策略的不断推行,人们的环保意识也在不断提升,但污染问题仍然时有发生。面对环境保护的需要,改进地下水中半挥发性有机化合物的测定方法是十分必要的。本文通过实验方法建立了固相萃取-气相色谱质谱法同时测定地下水中苯胺、阿特拉津、3,3'-二氯联苯胺的方法。检测方法为水样pH值为12,使用HLB小柱富集、正己烷洗脱后,通过固相萃取-气相色谱质谱法同时进行检测。苯胺方法检出限为0.66μg/L,atrazine方法检出限为0.82μg/L,3,3'-二氯联苯胺方法检出限为0.82μg/L。最低检测质量浓度分别为苯胺2.64μg/L,阿特拉津3.28μg/L,3,3'-二氯联苯胺3.28μg/L。在质量浓度范围内色谱峰面积在很大程度上呈线性相关,线性相关系数分别为0.9990、0.9985、0.9967。分别添加两浓度水平的苯胺、阿特拉津、3,3'-二氯联苯胺到水样中,平均加标回收率为51.7%~76.6%。该方法简洁快速,适用于地表水、地下水、工业废水和生活污水中半挥发性有机化合物的测定。

With the continuous implementation of the green development strategy,people’s awareness of environmental protection is also improving,but pollution problems still occur from time to time.Facing the need of environmental protection,it is necessary to improve the determination method of semi-volatile organic compounds in groundwater.A method for the simultaneous determination of aniline,atrazine and 3,3'-dichlorobenzidine in groundwater by solid phase extraction-gas chromatography-mass spectrometry has been established.The detection method is water sample pH=12,which is enriched with HLB small column and eluted with n-hexane,and then detected simultaneously by solid phase extraction and gas chromatography/mass spectrometry.The detection limit of aniline method is 0.66μg/L,the detection limit of atrazine method is 0.82μg/L,detection limit of 3,3'-dichlorobenzidine method is 0.82μg/L.The minimum detection mass concentration is 2.64 for anilineμg/L,atrazine 3.28μg/L,3,3'-dichlorobenzidine 3.28μg/L.In the range of mass concentration,the peak area of chromatography is linearly correlated to a large extent,and the linear correlation coefficients are 0.9990,0.9985 and 0.9967,respectively.Two concentration levels of aniline,atrazine and 3,3'-dichlorobenzidine were added to the water samples respectively,and the average recovery rate of spiking was 51.7%~76.6%.The method is simple and rapid,and is suitable for the determination of semi-volatile organic compounds in surface water,groundwater,industrial wastewater and domestic sewage.