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 chromatogra-phy-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 ultrasonica-tion 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,organic
solvents 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.
参考文献
| [1] | Hernandez F;Sancho JV;Pozo OJ.Critical review of the application of liquid chromatography/mass spectrometry to the determination of pesticide residues in biological samples[J].Analytical and bioanalytical chemistry,20054(4):934-946. |
| [2] | Chung, H.-W.;Ding, W.-H..Determination of organophosphate flame retardants in sediments by microwave-assisted extraction and gas chromatography-mass spectrometry with electron impact and chemical ionization[J].Analytical and bioanalytical chemistry,20097(7):2325-2334. |
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