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    超声辅助-分散液液微萃取-气相色谱-质谱法快速测定灰尘中多溴联苯醚

    Rapid Determination of Polybrominated Diphenyl Ethers in Dust by GC-MS Combimed with Ultrasonic Assisted Dispersion Liquid-Liquid Microextraction

    • 摘要: 0.100 0 g样品加入10 mL正己烷-丙酮(1+1)混合液中,于30℃超声提取20 min后,转移上清液,继续加10 mL正己烷-丙酮(1+1)混合液超声提取2次,合并上清液,用氮气吹至近干,加入5 mL水,混匀,用注射器快速注入0.75 mL丙酮和30 μL四氯化碳混合液,振荡数秒,以4 500 r·min-1转速离心5 min,取出沉积相,采用DB-5HT石英毛细管色谱柱(15 m×0.25 mm,0.1 μm)进行分离,质谱分析中采用电子轰击离子源和选择离子监测模式。7种多溴联苯醚的质量比均在一定范围内与对应的峰面积呈线性关系,方法检出限(3S/N)在0.90~10.0 mg·kg-1之间。加标回收率在61.3%~122%之间,测定值的相对标准偏差(n=6)在2.3%~12%之间。

       

      Abstract: The sample (0.100 0 g) was added into 10 mL of n-hexane-acetone (1+1) mixture for ultrasonic extraction at 30℃ for 20 min. After the supernatant was transferred, the sample was ultrasonically extracted twice with 10 mL of n-hexane-acetone (1+1) mixture. The combined supernatants were concentrated to nearly dry by nitrogen flowing, and 5 ml of water was added. After mixing well, a mixture of 0.75 mL of acetone and 30 μL of carbon tetrachloride were rapidly injected with a syringe, and the mixture was shaken for a few seconds and centrifuged at 4 500 r·min-1 for 5 min. The sedimentary phase was removed and separated on a DB-5HT quartz capillary column (15 m×0.25 mm, 0.1 μm). Electron impact ion source and selective ion monitoring mode were used for mass spectrometric analysis. Linear relationships were found between the peak area and the mass ratio of the 7 PBDEs in definite ranges. The detection limits (3S/N) were between 0.90 and 10.0 mg·kg-1. Values of recovery obtained by standard addition method were in ther range of 61.3%-122%, and the relative standard deviations (n=6) of the measured values were between 2.3% and 12%.

       

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