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摘要
A method was developed to determine phthalate esters in soil samples. The entire pre-treatment process involved microwave-assisted extraction, solvent conversion and clean-up of dispersive solid-phase extraction( DSPE). A total of 10 g soil sample was extracted by microwave mixed with 20 mL mixed-phase solvent of dichloromethane and acetone. And then the extract of mixed-phase was converted into the acetone-phase and then concentrated to 1.5 mL extract. The concentrated extract was shaken for 3 min that mixed with 0.2 g C-18 absorbent, and centrifuged for 10 min (8000 r/min). The supernatant (1.0 mL) was quantitatively transferred and converted into n-hexane phase. The entire clean-up process was lower than 20 min. 1.0 mL of the supernatant liquid was transferred into vial and then exchanged to hexane. Gas chromatography/mass spectrometry (GC/MS) was used for quantitative and confirmatory analysis of phthalate esters. The matrix effect of phthalate esters was compensated by matrix spiked calibration. The best removal efficiency of soil matrix was 72.65%. The method linearity range was 7.5-750 mu g/kg (r > 0.998). The RSDs of the actual soil samples and the spiked samples were 5.5% - 12.1% and 7.3% - 19.4%, respectively. The average recovery of the spiked samples was 94.4% - 114.6%, and the detection limit of the phthalate esters in soil samples was 1.2 - 4.3 mu g/kg.
- 出版日期2009-10
- 单位四川大学
