色谱
色譜
색보
CHINESE JOURNAL OF CHROMATOGRAPHY
2015年
8期
885-891
,共7页
王国光%张大海%杨丹丹%彭佳琳%李先国
王國光%張大海%楊丹丹%彭佳琳%李先國
왕국광%장대해%양단단%팽가림%리선국
超声辅助碱解萃取%气相色谱%电子捕获检测器%多溴联苯醚%海洋沉积物
超聲輔助堿解萃取%氣相色譜%電子捕穫檢測器%多溴聯苯醚%海洋沉積物
초성보조감해췌취%기상색보%전자포획검측기%다추련분미%해양침적물
ultrasonically assisted alkaline hydrolysis extraction%gas chromatography( GC)%electron capture detection( ECD)%polybrominated diphenyl ethers( PBDEs)%marine sedi-ments
将超声辅助碱液分解杂质与溶剂萃取相结合，采用气相色谱-电子捕获检测（ GC-ECD）建立了一种快速高效净化、萃取海洋沉积物中8种常见多溴联苯醚（ PBDEs）的分析方法。样品在2.00 mol／L NaOH 甲醇溶液中超声30 min，经正己烷萃取、单层硅胶净化、正己烷洗脱、旋蒸浓缩后定容至100μL，采用 GC-ECD 分析。结果表明， PBDEs各单体的加标回收率为63.6％~110.3％，相对标准偏差（ RSD）为1.7％~15.5％（ n=5）；十溴联苯醚（ BDE-209）的检出限为0.097 ng／g，其他7种单体的检出限为0.002~0.011 ng／g（信噪比为3）。该方法的准确度和精密度较高，稳定性和回收率良好，可满足沉积物中 PBDEs 的分析要求。利用建立的方法测定了渤海表层沉积物中PBDEs的含量，8种PBDEs总含量在1.566~6.760 ng／g之间，其中BDE-209的含量为1.461~6.438 ng／g，总体呈现出由近岸向远岸递减的趋势，表明人为活动、表层冲刷和陆地河流的输入对渤海地区 PBDEs 的含量有重要影响。
將超聲輔助堿液分解雜質與溶劑萃取相結閤，採用氣相色譜-電子捕穫檢測（ GC-ECD）建立瞭一種快速高效淨化、萃取海洋沉積物中8種常見多溴聯苯醚（ PBDEs）的分析方法。樣品在2.00 mol／L NaOH 甲醇溶液中超聲30 min，經正己烷萃取、單層硅膠淨化、正己烷洗脫、鏇蒸濃縮後定容至100μL，採用 GC-ECD 分析。結果錶明， PBDEs各單體的加標迴收率為63.6％~110.3％，相對標準偏差（ RSD）為1.7％~15.5％（ n=5）；十溴聯苯醚（ BDE-209）的檢齣限為0.097 ng／g，其他7種單體的檢齣限為0.002~0.011 ng／g（信譟比為3）。該方法的準確度和精密度較高，穩定性和迴收率良好，可滿足沉積物中 PBDEs 的分析要求。利用建立的方法測定瞭渤海錶層沉積物中PBDEs的含量，8種PBDEs總含量在1.566~6.760 ng／g之間，其中BDE-209的含量為1.461~6.438 ng／g，總體呈現齣由近岸嚮遠岸遞減的趨勢，錶明人為活動、錶層遲刷和陸地河流的輸入對渤海地區 PBDEs 的含量有重要影響。
장초성보조감액분해잡질여용제췌취상결합，채용기상색보-전자포획검측（ GC-ECD）건립료일충쾌속고효정화、췌취해양침적물중8충상견다추련분미（ PBDEs）적분석방법。양품재2.00 mol／L NaOH 갑순용액중초성30 min，경정기완췌취、단층규효정화、정기완세탈、선증농축후정용지100μL，채용 GC-ECD 분석。결과표명， PBDEs각단체적가표회수솔위63.6％~110.3％，상대표준편차（ RSD）위1.7％~15.5％（ n=5）；십추련분미（ BDE-209）적검출한위0.097 ng／g，기타7충단체적검출한위0.002~0.011 ng／g（신조비위3）。해방법적준학도화정밀도교고，은정성화회수솔량호，가만족침적물중 PBDEs 적분석요구。이용건립적방법측정료발해표층침적물중PBDEs적함량，8충PBDEs총함량재1.566~6.760 ng／g지간，기중BDE-209적함량위1.461~6.438 ng／g，총체정현출유근안향원안체감적추세，표명인위활동、표층충쇄화륙지하류적수입대발해지구 PBDEs 적함량유중요영향。
For determination of the eight polybrominated diphenyl ethers( PBDEs)in marine sediments based on gas chromatography-electron capture detection( GC-ECD ),a rapid and effective method for simultaneous sample extraction and purification was developed,in which ultrasonically assisted alkaline hydrolysis was combined with solvent extraction. The sediment sample was processed in an ultrasonic bath in 2. 00 mol/L NaOH-methanol solution for 30 min, and subsequently extracted by n-hexane. The organic phase was then separated and purified by silica column and concentrated to 100 μL for GC-ECD analysis. Under the optimized conditions, the recoveries and relative standard deviations( RSDs)for eight PBDE congeners ranged from 63. 6% to 110. 3% and from 1. 7% to 10. 5%( n = 5 ),respectively. The limits of detection ( LODs,S/N=3)ranged from 0. 002 to 0. 011 ng/g except for deca-brominated diphenyl ether ( BDE-209),which was 0. 097 ng/g. With high accuracy,good stability and adequate recovery, the established method was successfully applied to the analysis of PBDEs in the surface sedi-ments from Bohai Sea. The concentrations of ∑8PBDEs(sum of 2,4,4′-tribromodiphenyl ether ( BDE-28),2,2′,4,4′-tetrabromodiphenyl ether( BDE-47 ),2,2′,4,4′,5-pentabromodiphenyl ether ( BDE-99 ), 2,2′,4,4′,6-pentabromodiphenyl ether ( BDE100 ), 2,2′,4,4′,5,5′-hexabromodiphenyl ether( BDE-153),2,2′,4,4′,5,6′-hexabromodiphenyl ether( BDE-154), 2,2′,3,4,4′,5′,6-heptabromodiphenyl ether( BDE-183),BDE-209)and BDE-209 ranged from 1. 566 to 6. 760 ng/g and from 1. 461 to 6. 438 ng/g,respectively. A decreasing gradient of con-centration was basically observed with increasing distance off the shore ,indicating that anthro-pogenic activities,surface runoff and river inputs may be the sources of PBDEs in the sedi-ments from Bohai Sea.
