Determination of alkylphenols and bisphenol A in sediment by gas chromatography-mass spectrometry
A method was developed for the simultaneous determination of 8 trace APs and BPA in sediments by accelerated solvent extraction,silica gel column purification and gas chromatography-mass spectrometry.After freeze-drying,the samples were extracted with acetone-dichloromethane(V/V=1/2)as the extraction solvent under 100℃.The extracts were purified by silica gel column,separated by gas chromatography and detected by mass spectrometry,qualitatively determined according to retention time,mass spectrum and abundance of fragments,and quantified by internal standard methods.The results showed that the target compounds showed a good linear relationship in the range of 10-2000 μg·L-1,and the correlation coefficients were greater than 0.9994,and the limits of detections(LODs)were between 0.6 and 1.9 μg·kg-1.The relative standard deviations(RSDs,n=7)of the compounds in 200 μg·L-1 and 500 μg·L-1 standard solutions were in the range of 1.9%-5.4%,and the spiked recoveries were in the range of 85.7%-99.5%.And the method was applied to the detection of sediment samples from a river in Tianjin.And 4-butylphenol,4-tert-octylphenol,4-nonylphenol and bisphenol A were detected.In addition,the spiked recoveries of APs and BPA in the actual samples were in the range of in the range of 84.5%-97.4%.The results show that this method was simple,high in sensitivity and recoveries,good in accuracy and reproducible,and could meet the requirements of trace APs and BPA detection in sediment samples.
Gas chromatography-mass spectrometryalkylphenolsbisphenol asediment