超声提取/固相萃取测定固体介质中合成麝香及有机磷酸酯阻燃剂/增塑剂

Determination of Synthetic Musks and Organophosphate Flame Retardants/Plasticizers in Solid Phase by Ultrasound-assisted Extraction Coupled with Solid Phase Extraction

基于超声提取与固相萃取技术,建立了沉积物和污泥中合成麝香与有机磷酸酯增塑剂/阻燃剂联合前处理方法,并采用气相色谱-质谱对目标化合物进行定性定量分析。考察了不同溶剂对目标化合物萃取效率的影响,确定以丙酮与乙腈-水(1∶3)的组合作为超声萃取溶剂。研究了基质效应和老化效应对目标化合物回收率的影响。结果表明,不同加标浓度下,4种常见合成麝香和9种常用有机磷酸酯的回收率为(27%±12%)^(117%±9%)。

A rapid method was developed for the simuhaneous determination of synthetic musks and organophosphate esters （OPs） in sediment/sludge, based on ultrasonic-assisted extraction, solid phase extraction（SPE） and the subsequent analysis by gas chromatography -mass spectrometry （GC - MS）. In this study, different solvents were investigated and optimized, and thus acetone and ace- ied. Under the optimized conditions, 13 analytes including 9 widely used OPs and 4 synthetic musks were extracted and analyzed, and the results indicated that acceptable recoveries of the analytes were achieved in the range of （27% ± 12% ） - （117% ±9% ）, from sediment, sludge and pre-extracted sediment at different spiked concentrations.