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.