Citation:
LIU Shi-Long, ZHANG Hua, HU Xiao-Hui, QIU Yan-Ling, ZHU Zhi-Liang, ZHAO Jian-Fu. Analysis of Organophosphate Esters in Sediment Samples Using Gas Chromatography-Tandem Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry,
;2016, 44(2): 192-197.
doi:
10.11895/j.issn.0253-3820.150600
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An efficient extraction and purifying method coupled to gas chromatography-tandem mass spectrometry (GC-MS/MS) with electron impact (EI) detection was developed to determine eight organophosphate esters (OPEs) in sediment samples. The selected OPEs were extracted twice from the sediments through vortex oscillation and ultrasonic extraction using 20 mL of n-hexane and acetone mixture (1:1, V/V) for 10 min. Further purification by Florisil solid phase extraction (SPE) column, elution by 8 mL of ethyl acetate, concentration, and solvent exchanges for n-hexane were carried out. All target compounds were separated using the DB-5ms capillary column (30 m×0.25 mm×0.25 μm) and detected by tandem mass spectrometry with selected reaction monitoring, and determined by the internal standard method. The result showed that this pretreatment method was simple with less solvent consumption. At three spiked levels of 10, 20 and 50 μg/L, the recovery of selected OPEs (except TEP) was 80% to 120%, and the limit of detection was 0.31-64.5 ng/L, showing a good precision and accuracy.
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