A method was established for the determination of four new pollutants(4-Nonylphenol,2,4-Trichlorothiramate,Trichlorothiramate,1,2,5,6,9,10-Hexabromocyclododecane)in soil and sediment using ASE extraction-Modified QuEChERS purification-GCMS.Ten grams of soil or sediment samples were extracted with a mixture of V(n-hexane)∶V(acetone)=1∶1 as the extraction solvent.The extraction was performed at 100℃for 2 minutes with two static extractions.The extract was dehydrated with anhydrous sodium sulfate,purified with 20 mg of N-propylethylenediamine(PSA)and 10 mg of reduced graphene oxide,and then vortexed,centrifuged,and made up to a constant volume.The separation was achieved on a DB-5MS column(30 m×0.25 μm× 0.25 mm),and the qualitative and quantitative analysis was performed using gas chromatography-mass spectrometry with an electron impact ionization source(EI)and selected ion monitoring(SIM)mode with the internal standard method.The results showed that the four new pollutants showed good linearity within the mass concentration range of 0.1～1.0 mg/L,with correlation coefficients(r)all greater than 0.998.The detection limits for soil and sediment samples were 0.8～2.0 μg/kg and 1.2～2.4 μg/kg,respectively.The limits of quantitation were 3.2～8.0 μg/kg and 4.8～9.6 μg/kg,respectively.The method was applied to analyze soil and sediment samples collected around a pesticide factory,and three pesticides,namely trichlorfon,4-nonylphenol,and 1,2,5,6,9,10-hexabromocyclododecane,were detected at different concentrations,with a detection rate of 14.1％.
关键词
新污染物/土壤/沉积物/加压流体萃取/QuEChERS/气相色谱质谱联用
Key words
new pollutants/soil/sediment/accelerated solvent extraction/QuEChERS/GC-MS
维普
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