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建立水中13种多溴联苯醚(Polybrominated diphenyl ethers,PBDEs)固相(solid-phase extraction,SPE)萃取-气相色谱分析方法。水样经弗罗里硅土(Florisil)固相萃取柱富集后,用2 mL正己烷和5 mL正己烷:二氯甲烷(V∶V=8∶2)进行洗脱,采用HP-5(30 m×320μm×0.25μm)毛细管柱分离,气相色谱仪(GC-uECD)检测。结果表明,在0.05、0.25、0.5μg/L3个添加水平中,13种PBDEs的平均添加回收率在67.9%~121.5%的范围内,相对标准偏差为2.5%~12.3%。其中BDE-209的平均添加回收率为67.9%~71.9%,相对标准偏差为5.2%~8.0%。BDE-209的方法检出限是1.2 ng/L;其余12种PBDEs的方法检出限是0.11~0.5 ng/L。该方法准确度较高;稳定性和回收率良好;可测定多组分PBDEs,满足环境样品中PBDEs的分析。
A method for the determination of thirteen Polybrominated diphenyl ethers (PBDEs) in water by solid-phase extraction (SPE) and gas chromatography was established. The sample was concentrated on a Florisil SPE cartridge and eluted with 2 mL of n-hexane and 5 mL of n-hexane: dichloromethane (V: V = 8: 2) (30 m × 320 μm × 0.25 μm) capillary column and gas chromatography (GC-uECD). The results showed that the average recoveries of 13 PBDEs ranged from 67.9% to 121.5% with relative standard deviations of 2.5% to 12.3% at 0.05, 0.25 and 0.5 μg / L. The average recoveries of BDE-209 were 67.9% -71.9% with relative standard deviations of 5.2% -8.0%. The detection limit of BDE-209 was 1.2 ng / L. The detection limits of the other 12 PBDEs ranged from 0.11 to 0.5 ng / L. The method has high accuracy, good stability and recovery, and can measure multi-component PBDEs to meet the analysis of PBDEs in environmental samples.