超声萃取-气相色谱-质谱联用测定海洋沉积物中39种多溴联苯醚残留

Determination of 39 Polybrominated Diphenyl Ethers in Coastal Sediments by Ultrasonic Extraction Coupled with Gas Chromatography-Mass Spectrometry

建立了超声萃取-气相色谱-质谱法测定海洋沉积物中39种多溴联苯醚残留的分析方法。样品用V(正己烷)∶V(二氯甲烷)=1∶1混合溶液提取,超声(控制水浴温度为25℃)提取60min,采用硅胶和氧化铝净化,负化学离子源-气相色谱-质谱法进行检测,39种组分图谱在49min内能得到很好的分离。39种混合样品的检出限为0.003～0.10μg/kg;加标回收率为66.2%～118.6%;相对标准偏差为0.8%～18.2%。用于实际样品分析,结果令人满意。

A method was developed for the determination of 39 polybrominated diphenyl ethers （PBDEs） from mono-to hepta-brominated in coastal sediment by gas chromatography/mass spectrometry. The sample was extracted with a solution of dichloromethane： n-hexane （1：1, V/V）, followed by ultrasonic extraction for 60 min at 25 ℃. The clean-up step was optimized using silica gel and alumina. The detection limit of the method was in the range of 0.003 -0.10 μg/kg. The results indicate that the average recovery of the internal standard was from 66.2% to 118.6%. The relative standard deviation RSD（%） was from 0.8 % to 18.2%. The method for the detection of 39 PBDE congeners in coastal sediment was sensitive, high reproducible with satisfactory recoveries.