Preconcentration sensitive determination of pyrethroid insecticides in environmental water samples with solid phase extraction with SiO_2 microspheres cartridge prior to high performance liquid chromatography

摘要

Present study developed a new method for the sensitive determination of pyrethroid insecticides with solid phase extraction in combination with high performance liquid chromatography and UV detector. SiO_2 microspheres, a new SiO_2 based material, was investigated for the enrichment ability and applicability as the solid phase extraction sorbent. Four pyrethroid pesticides such as fenpropathrin, cyhalothrin, fenvalevate and biphenthrin were used as the target analytes. Parameters that maybe influence the extraction efficiency such as the eluent type and its volume, sample flow rate, sample pH, and the sample volume were optimized in detail, and the optimal conditions were as followed: sample volume, 100mL; concentration of methanol, 30%; acetone volume, 5mL; sample flow rate, 4.2mLmin~(-1); sample pH, 7. The experimental results indicated that there was good linearity in the concentration range of 0.1-50μgL~(-1) except biphenthrin in the range of 0.05-25μgL~(-1). The detection limits for fenpropathrin, cyhalothrin, fenvalevate and biphenthrin were in the range of 0.02-0.08μgL~(-1). The intra-day and day to day precisions (RSDs, n=6) were in the ranges of 2.6-4.4% and 5.3-7.2%, respectively. The method was validated with five real environmental water samples, and all these results proved that proposed method could be used as a good alternative for the routine analysis for such pollutants in environmental samples.