摘要
建立了测定松针样品中多溴联苯醚（PBDEs）的分析方法。松针样品经过正己烷．丙酮（体积比为1：1）混合溶液超声萃取、浓硫酸和氧化铝柱净化后，采用气相色谱-负化学电离源质谱（GC—NCI—MS）选择离子监测（SIM）模式检测，内标法定量。结果表明，方法的加标回收率为83．8％～107．5％，三溴-七溴代联苯醚的仪器检出限为0．152～0．770pg，十溴代联苯醚（BDE-209）的检出限为11．1pg；三溴-七溴代联苯醚的方法检出限（湿重）为3～15pg／g，BDE-209的方法检出限（湿重）为222pg／g。方法具有良好的重现性、较高的灵敏度和良好的回收率。实际样品分析表明，松针中BDE-209是主要的同类物，约占8种PBDEs总量的82．3％，低溴代联苯醚以2，2’，4，4’-四溴联苯醚（BDE-47）为主。
A method for the determination of polybrominated diphenyl ethers （PBDEs） in pine needles was developed. Ultrasonic-assisted extraction （UAE） was employed with n-hexane-acetone （1： 1, v/v）, and concentrated H2SO4 and an alumina column were used for cleaning-up the extract of pine needles. The final extract was identified and quantified for the 8 PBDE congeners （BDE-28, 47, 99, 100, 153, 154, 183, and 209） by gas chromatography-negative chemical ionization-mass spectrometry （GC-NCI-MS） with internal standard method in the selective ion monitoring （SIM） mode. The recoveries of the spiked standards ranged from 83.8% to 107.5%. The instrumental detection limits for tri- to hepta-BDEs （BDE-28, 47, 99, 100, 153, 154 and 183） were in the range of 0. 152 -0.770 pg, and for BDE-209 was 11. 1 pg. The method detection limits for the above-mentioned PBDEs were 3 - 15 pg/g wet weight and 222 pg/g wet weight, respectively. The results indicate that the me.thod has high sensitivity, satisfactory recovery and good repro- ducibility. BDE-209 was found to be the dominant congener （82.3% of the total of 8 PBDEs）, and BDE-47 was the major congener among the lower brominated congeners.
出处
《色谱》
CAS
CSCD
北大核心
2009年第1期59-62,共4页
Chinese Journal of Chromatography
基金
国家重点基础研究计划("973"计划)课题(2006CB403302)
关键词
超声辅助萃取
气相色谱-负化学电离源质谱
多溴联苯醚
松针
ultrasonic-assisted extraction （UAE）
gas chromatography-negative chemical ionization-mass spectrometry （GC-NCI-MS）
polybrominated diphenyl ethers （PBDEs）
pine needles
