|
| Simultaneous Determination of 13 Organophosphate Esters in Greenhouse Soil by Gas Chromatography-Mass Spectrometry |
| |
| View Full Text Download reader |
| DOI： |
| KeyWord:ultrasonic extraction gas chromatography-mass spectrometry(GC-MS) organophosphate esters greenhouse soil |
| Author | Institution |
| SANG Yong-zhu,LI Wen-hui,LIU Jie-min,QU Chen,ZHAO Yan-jun,CAI Han-mei,HONG Si-cheng |
1.National Standard Beijing Inspection and Certification Co.,Ltd.;2.School of Chemistry and Biological Engineering,University of Science and Technology Beijing;3.China Building Materials Testing and Certification Group Co.,Ltd. |
|
| Hits: 1616 |
| Download times: 676 |
| Abstract: |
| In this study,a gas chromatography-mass spectrometry(GC-MS) was developed for the simultaneous detection of 13 kinds of organophosphate esters(OPEs) in greenhouse soil,including triethyl phosphate,tripropyl phosphate,tri-n-butyl phosphate,triisobutyl phosphate,tributoxyethyl phosphate,tris(2-ethylhexyl) phosphate,tris(2-chloroethyl) phosphate,tris(1-chloro-2-propyl) phosphate,Tris(1,3-dichloro-2-propyl) phosphate,triphenyl phosphate,tricresyl phosphate,toluene diphenyl phosphate and 2-ethylhexyl diphenyl phosphate.The experimental parameters such as extraction solvents,extraction methods,extraction times,extraction column types and chromatographic conditions were optimized.The soil samples were ultrasonically extracted with n hexane-acetone(1∶1,by volume),and then purified with a Florisil solid phase extraction column,followed by analysis of GC-MS in selected ion monitoring mode and quantitative analysis by internal standard method.Results showed that there were good linear relationships for 13 target compounds in the mass concentration range of 1-500 μg/L,with their correlation coefficients(r2) of 0.999 3-0.999 7.The limits of detection(LODs,S/N=3) and limits of quantitation(LOQs,S/N=10) were in the ranges of 0.04-2.31 μg/L and 0.13-7.69 μg/L,respectively.The soil spiked recoveries at three spiked levels of 1.0,10 and 50 μg/L ranged from 54.5% to 130%,with relative standard deviations(RSDs) of 1.7%-9.9%.This method was applied to the analysis of 41 soil samples from vegetable greenhouses in Beijing.Except for tripropyl phosphate,12 kinds of OPEs were detected in all samples,with the concentration range of 1.90-632 ng/g(dry weight,dw),the mean value of 87.8 ng/g and the median value of 39.7 ng/g.Tributyloxyethyl phosphate is the most abundant OPEs,contributing about 20% of the total content of 12 kinds of organophosphate esters(∑12OPEs).This method is simple,rapid,sensitive and accurate,and could meet the demands for analysis of 13 OPEs in soil. |
| Close |
|
|
|