超声辅助萃取-气相色谱-负化学电离源质谱法测定室内灰尘样品中8种常见多溴联苯醚

摘要

A method for the determination of eight polybrominated diphenyl ethers (PBDEs) in indoor dust was developed. A vacuum cleaner was used for gathering the house dust, and n-hexane was added and the extraction was performed in an ultrasonic bath. The supernatant was concentrated and then n-hexane was added to 0. 1 mL. Gas chromatography-negative chemical ionization mass spectrometry (GC-NCI/MS) has been investigated for the determination of the eight PBDE congeners in indoor dust. The eight PBDEs were separated within 20 min. The absolute recoveries were 53. 2% - 107. 6%. The relative standard deviations (RSDs) of intra-day were between 2. 8% and 16. 5%, while the RSDs of inter-day were between 6. 4% and 22. 6%. The limits of detection (LOD, S/N = 3) were in the range of 0. 003 - 0. 015 ng/g except the LOD of BDE-209 was 0. 15 ng/g. The results indicated that the proposed method is sensitive, accurate , fast, simple, low solvent consumption and suitable for the determination of tri- to deca-BDEs in indoor dust.%建立了室内灰尘样品中8种常见多溴联苯醚(PBDEs:BDE-28、BDE-47、BDE-99、BDE-100、BDE-153、BDE-154、BDE-183和BDE-209)的气相色谱-负化学电离源质谱(GC-NCI/MS)分析方法.样品经吸尘器采集、正己烷超声萃取、浓缩后,采用GC-NCI/MS测定.结果表明,方法的加标回收率为53.2％ ～107.6％,日内测定的相对标准偏差(RSD)为2.8％～16.5％,日间测定的RSD为6.4％～22.6％.除了BDE-209的检出限(信噪比为3)为0.15ng/g外,其他多溴联苯醚的检出限为0.003～0.015 ng/g.该方法灵敏度高,准确度和精密度好,简便快速,溶剂消耗量少,适用于灰尘中三溴～十溴联苯醚的测定.