加速溶剂萃取-液相色谱-串级质谱法测定近岸及河口沉积物中的拟除虫菊酯农药

摘要

A rapid and accurate method was developed for the measurement of 12 pyrethroid pesticides in estuarine and coastal sediments by accelerated solvent extraction (ASE) and liquid chromatography-tandem mass spectrometry (LC-MS/MS). The pyrethroid pesticides were extracted in 5.0 min and repeated one more time by ASE using mixed solvent of n-hexane and acetone(1:1, V/V) at 60 degrees C and pressure of 10.3 MPa with static extraction mode. After concentrated, the pesticides were separated with XDB-C-18 column with mobile phase of methanol and water containing 2.5 mmol/L ammonium acetate, and then determined with tandem mass spectrometer using positive ESI at MRM mode. Under the optimized conditions, relative standard deviation( RSD) for developed method was 1.1% 8.6% (20.0 mu g/kg, n = 8), standard added recoveries were 67.9% - 97.3%, and the limits of quantification(LOQ, 10 sigma) were 0.5 - 2.5 mu g/kg.