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| Determination of Estrogens in Sewage Sludge by Matrix Dispersion Solid-phase Extraction with High Performance Liquid Chromatography-Tandem Mass Spectrometry |
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| DOI：10.3969/j.issn.1004-4957.年份.月份 |
| KeyWord:estrogens sewage sludge matrix solid-phase dispersion extraction(MSPD) high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS） |
| Author | Institution |
| ZHAO Xin,ZHANG Zhan-en,ZHANG Lei,PENG Shu-xiang,CHENG Hao |
1.苏州科技学院环境科学与工程学院;2.苏州科技学院江苏省环境科学与工程重点实验室 |
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| Abstract: |
| A matrix solid-phase dispersion（MSPD） with high performance liquid chromatography tandem mass spectrometric（HPLC-MS/MS） method was established for the simultaneous determination of six estrogens（estriol,estradiol,17α-ethinylestradiol,estrone,diethylstilbestrol and bisphenol A） in sewage sludge.The 0.3 g sewage sludge sample was mixed with 1.5 g Florisil for matrix solid phase dispersion by using the new grinding method,then the mixed sample was transferred to a column and eluted with 6 mL methanol.The eluent was purified by dispersive solid phase extraction（DSPE） using HC-C18 as cleaning agent,and then concentrated to 0.6 mL by nitrogen.The six estrogens were separated upon a Syncronis C18 column using acetonitrile-water as mobile phase by gradient elution,and detected by MS under selected reaction monitoring（SRM） mode.The external standard method was used for quantitation analysis.The results indicated that six target estrogens can achieve the good linearities in the range of 1-50 μg?kg-1,with correlation coefficients higher than 0.992.The limits of detection（LODs） for the target compounds ranged from 0.12 μg?kg-1 to 0.25 μg?kg-1.Average recoveries of 6 analytes at three spiked levels ranged from 81.4% to 107.3% with relative standard deviations（RSDs） of 1.8%-9.7%.The developed method was applied in the analysis of 6 estrogens in sewage sludge samples from two sewage treatment plants in Suzhou,of which 5 target compounds except diethylstilbestrol were detected with concentration of 1.08-24.3 μg?kg-1.The method was rapid,sensitive and reliable,and was suitable for the simultaneous determination of trace estrogen in sewage sludge. |
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