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  

Determination of polybrominated diphenyl ethers in indoor dust using ultrasonic-assisted extraction and gas chromatography-negative chemical ionization mass spectrometry

作　　者：张晓玲[1] 王炳玲[2] 陆晓梅[1] 张琦[2] 张正东[2] 

机构地区：[1]南京医科大学公共卫生学院卫生检验学系,江苏南京210029 [2]南京医科大学公共卫生学院职业医学与环境卫生学系,江苏南京210029

出　　处：《色谱》2012年第12期1241-1245,共5页Chinese Journal of Chromatography

基　　金：国家自然科学基金面上项目(81072268);江苏省自然科学基金面上项目(BK2010535);江苏省博士后基金项目(1001017C);江苏高校优势学科建设工程资助项目

摘　　要：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0.15 ng/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。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.

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 室内灰尘 

分 类 号：O658[理学—分析化学]