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Optimization of selective pressurized liquid extraction and ultrasonication-assisted QuEChERS methods for the determination of polybrominated diphenyl ethers in sediments

机译:选择性加压液体萃取和超声辅助QuEChERS方法测定沉积物中多溴联苯醚的优化

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Two fast analytical methods, selective pressurized liquid extraction (SPLE) and ultrasonication-assisted QuEChERS methods (Quick, Easy, Cheap, Effective, Rugged and Safe) followed by GC-MS/MS, were optimized for the determination of polybrominated diphenyl ethers (PBDEs) in sediments. Ultrasonication was used to improve the extraction efficiency of QuEChERS. The experimental parameters of SPLE and ultrasonication-assisted QuEChERS, such as sorbent type, composition and elution solvents, were optimized in detail. The obtained recoveries of both methods were satisfactory for PBDE analysis. The inter/intra-day RSDs were 7%. The limits of quantification (LOQ) were a‰¤0.1 ng ga?’1 dry weight (d.w.). The figures of merit were at the same level as former reported results. The proposed methods were validated for the analysis of PBDEs in standard reference materials (SRM 1944 and 2585). The results indicated that both optimized methods were feasible for the analysis and monitoring of PBDEs. Besides, the comparison between two methods revealed that elevated temperature and pressure could weaken the interaction between PBDEs and sediment matrices, resulting in improvement of extraction efficiency. Both proposed methods were successfully applied to the analysis of 3 sediment samples and the determination of BDE 47, 99, 100 and 153 suggested that both methods are practical and suitable for PBDE analysis in real sediment samples.
机译:优化了两种快速分析方法,分别是选择性加压液体萃取(SPLE)和超声辅助QuEChERS方法(快速,简便,廉价,有效,坚固和安全),然后是GC-MS / MS,用于测定多溴联苯醚(PBDEs) )在沉积物中。超声处理可提高QuEChERS的提取效率。详细优化了SPLE和超声辅助QuEChERS的实验参数,例如吸附剂类型,组成和洗脱溶剂。两种方法的回收率均令人满意,适用于多溴二苯醚分析。日间/日内RSD均小于7%。定量极限(LOQ)为±0.1 ng ga?-1干重(d.w.)。绩效指标与先前报告的结果处于同一水平。验证了所提出的方法用于分析标准参考物质(SRM 1944和2585)中的多溴二苯醚。结果表明,两种优化方法对多溴二苯醚的分析和监测都是可行的。此外,两种方法的比较表明,高温和高压会削弱多溴二苯醚与沉积物基质之间的相互作用,从而提高萃取效率。两种方法都成功地用于3种沉积物样品的分析,BDE 47、99、100和153的测定表明这两种方法都是实用的,适用于实际沉积物样品中的PBDE分析。

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