以沉积物和污泥中非极性和弱极性有机污染物的非靶标筛查为目的,建立了一种超声波辅助提取-气相色谱-质谱结合自动解卷积技术的筛查方法。以二氯甲烷为溶剂超声波辅助提取样品3次,每次20 min,提取液经凝胶渗透色谱(GPC)和硅胶层析柱净化,再用3 g铜粉超声10 min除硫。前处理方法的重复性(RSD,n=5)为5.8%~14.9%。采用自动质谱解卷积软件(AMDIS)和标准谱库定性鉴别出所含的有机物。在两类样品中共鉴别出290种有机污染物,其中沉积物样品中190种,污泥样品中153种。鉴别出的污染物包括美国环境保护署(EPA)优先控制污染物、药物和除草剂等新型污染物、抗氧化剂、中间体、有机溶剂及化工原料等。该方法灵敏度高,重复性好,可用于复杂基质样品中有机污染物的非靶标筛查。
A screening method in the combination of ultrasonic extraction,gas chromatography-mass spectrometry detection and automated mass spectrometry deconvolution technique was developed for non-target screening of non-polar and weak polar pollutants in sediments and sludges. The samples were extracted by ultrasonication for 20 min using dichloromethane for three times. The extraction solutions were cleaned-up by gel permeation chromatography and a silica gel column,and then 3 g of copper powder was used to remove the sulfur by ultrasonication for 10 min. Parallel experiments were carried out for 5 times and the RSDs were ranged from 5. 8% to 14. 9%. Automated mass spectral deconvolution identification system(AMDIS)would improve the resolution of overlapping peaks,and identify the pure mass spectrum of the analytes in the cases of stronger background interference and co-extracted substances covering.Standard spectrum databases,such as NISTDRUG,NISTEPA,NISTFDA,Mass Spectral Library,etc,would qualitatively identify the organic pollutants in the samples. As a result,a total of 290 organic pollutants were identified,of which 190 and 153 pollutants were found in sediments and sludges,respectively. The identified pollutants included the Environmental Protection Agency(EPA)priority pollutants,pharmaceuticals,herbicides,antioxidants,intermediates,organicsolvents and chemical raw materials. The proposed method is proved to be a promising one for non-target screening of complex matrix samples with the advantages of higher sensitivity and better repeatability.