水样中痕量十溴联苯醚的分散液-液微萃取条件的优化

采用正交设计和Box-Penhnken响应面设计,对分散液-液微萃取技术萃取水样中痕量十溴联苯醚的条件进行了筛选和优化,得到最佳条件:四氯乙烯为萃取剂(10μl)、丙酮作分散剂(1ml)、pH范围5~9、离子强度,2%NaCl及萃取时间10min。此优化条件下分散液-液微萃取技术的萃取回收率可达92.37%~104.38%,富集倍数为508~611。优化条件下方法的线性范围为0.01~100ng/ml,检出限(S/N=2)为3.0pg/ml,加标回收率为96.25%~102.16%,精密度为5.44%~6.34%。

Optimization of Dispersive Liquid-liquid Microextraction for Decabrominated Diphenyl Ether at Trace Level in Water Sample

Conditions of dispersive liqiuid-liquid microextraction (DLLME) for decabrominated diphenyl ether (decaBDE) at trace level in water sample was investigated and optimized using the multi-factorial orthogonal design and Box-benhnken design. The optimal conditions were obtained as follow: 10μl of extraction solvent ( tetrachloroethylene), disperser solvent (acetone) of 1ml, NaCl of 2 % (ionic strength), pH 5～9, and extraction time of 10min, and validated through the measurement of decabrominated diphenyl ether added in real water samples at different levels. The extraction recovery (ER) was between 92.37% and 104.38%, and enrichment factor (EF) was from 508 to 611. The proposed method exhibited a wide linear range (0.05～100ng/mL) under the optimal conditions. The limit of deteetian (LOD) was 3.0 pg/mL (S/N = 2), the recoveries were range from 96.25% to 102.16%, and RSDs (n = 3) range was 5.44～6.34.