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.
Simultaneous Determination of 12 Organophosphate Esters in Soil by Solid Phase Extraction/High Performance Liquid Chromatography-Tandem Mass Spectrometry
Determination on Ultra-trace of Polycyclic Aromatic Hydrocarbons in Atmospheric Particulate Matters by Liquid Chromatography Coupled with Ultrasonic Extraction and Online Solid Phase Extraction Concentration
Determination of Quinoline and Isoquinoline in Textiles by Gas Chromatography-Mass Spectrometry
Determination of 16 Polycyclic Aromatic Hydrocarbons in Alpinia Oxyphylla Miq by Gas Chromatography-Mass Spectrometry
Detection of Phospholipid Compounds in Soybean and Soybean Oil Samples Using Ultrasonic Extraction and Normal phase HPLC with UV Detection
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School of Environmental Science and Engineering,Southern University of Science and Technology
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