色谱
色譜
색보
Chinese Journal of Chromatography
2015年
10期
1071-1079
,共9页
郑晓燕%于建钊%许秀艳%于海斌%陈烨%谭丽%吕怡兵
鄭曉燕%于建釗%許秀豔%于海斌%陳燁%譚麗%呂怡兵
정효연%우건쇠%허수염%우해빈%진엽%담려%려이병
同位素稀释-高分辨气相色谱/高分辨质谱%多溴联苯醚%多溴联苯153%大气%环境监测
同位素稀釋-高分辨氣相色譜/高分辨質譜%多溴聯苯醚%多溴聯苯153%大氣%環境鑑測
동위소희석-고분변기상색보/고분변질보%다추련분미%다추련분153%대기%배경감측
isotope dilution-high resolution gas chromatography/high resolution mass spectrometry%polybrominated diphenyl ethers (PBDEs )%polybrominated biphenyls 153 (BB153)%ambient air%environmental monitoring
针对环境监测的特点和要求,建立了同位素稀释-高分辨气相色谱/高分辨质谱测定大气中多溴联苯醚( PBDEs)和多溴联苯153( BB153)的方法。采用正己烷/二氯甲烷(1:1,v/v)及正己烷分别对 PBDEs 和 BB153进行快速溶剂萃取,并通过复合硅胶柱净化。在校准曲线最高浓度的10%和90%加标水平下得到的天然内标的平均回收率分别为100%和104%,平均相对标准偏差( n=7)分别为5%和6%;二至十溴代联苯醚和BB153相应的13 C同位素标准物质回收率在36.5%~133%之间;而一溴代联苯醚13 C同位素标准物质回收率较差,可能是由于物化性质与其他化合物不同。在实际采样体积为300 m 3的情况下,未发生污染物穿透现象;分析物检出限低于2×10-4 ng/Nm3,提取内标回收率在56%~126%之间(一溴代联苯醚除外)。实验结果表明该方法能对化合物准确定量,适用于大气中二至十溴代联苯醚和 BB153的分析。
針對環境鑑測的特點和要求,建立瞭同位素稀釋-高分辨氣相色譜/高分辨質譜測定大氣中多溴聯苯醚( PBDEs)和多溴聯苯153( BB153)的方法。採用正己烷/二氯甲烷(1:1,v/v)及正己烷分彆對 PBDEs 和 BB153進行快速溶劑萃取,併通過複閤硅膠柱淨化。在校準麯線最高濃度的10%和90%加標水平下得到的天然內標的平均迴收率分彆為100%和104%,平均相對標準偏差( n=7)分彆為5%和6%;二至十溴代聯苯醚和BB153相應的13 C同位素標準物質迴收率在36.5%~133%之間;而一溴代聯苯醚13 C同位素標準物質迴收率較差,可能是由于物化性質與其他化閤物不同。在實際採樣體積為300 m 3的情況下,未髮生汙染物穿透現象;分析物檢齣限低于2×10-4 ng/Nm3,提取內標迴收率在56%~126%之間(一溴代聯苯醚除外)。實驗結果錶明該方法能對化閤物準確定量,適用于大氣中二至十溴代聯苯醚和 BB153的分析。
침대배경감측적특점화요구,건립료동위소희석-고분변기상색보/고분변질보측정대기중다추련분미( PBDEs)화다추련분153( BB153)적방법。채용정기완/이록갑완(1:1,v/v)급정기완분별대 PBDEs 화 BB153진행쾌속용제췌취,병통과복합규효주정화。재교준곡선최고농도적10%화90%가표수평하득도적천연내표적평균회수솔분별위100%화104%,평균상대표준편차( n=7)분별위5%화6%;이지십추대련분미화BB153상응적13 C동위소표준물질회수솔재36.5%~133%지간;이일추대련분미13 C동위소표준물질회수솔교차,가능시유우물화성질여기타화합물불동。재실제채양체적위300 m 3적정황하,미발생오염물천투현상;분석물검출한저우2×10-4 ng/Nm3,제취내표회수솔재56%~126%지간(일추대련분미제외)。실험결과표명해방법능대화합물준학정량,괄용우대기중이지십추대련분미화 BB153적분석。
Considering the features and demands of the environmental monitoring,an isotope dilution-high resolution gas chromatography/high resolution mass spectrometry method was developed for the determination of polybrominated diphenyl ethers( PBDEs)and polybrominat-ed biphenyls 153( BB153)in the ambient air. PBDEs and BB153 were extracted using an accel-erated solvent extraction apparatus with a mixture of hexane-dichloromethane( v/v,1:1)and hexane,respectively. The concentrated extracts were loaded on the composite silica gel column for cleanup. The mean recoveries of native compounds at 10% and 90% of the highest levels of calibration curves were 100% and 104% with 5% and 6% of the mean relative standard devia-tions(n=7),respectively. The recoveries of 13C labeled surrogates for di- to deca-brominated diphenyl ethers and BB153 were in the range of 36. 5%-133%. However,the recoveries of 13C-monobrominated diphenyl ethers were relatively low ,maybe due to the different physicochemi-cal properties compared with the other homologues. No breakthrough of pollutants was esti-mated under real sampling volume of 300 m 3 . The limits of detection were lower than 2 × 10-4 ng/Nm3. The recoveries of 13C labeled surrogates were between 56% and 126%, except monoBDEs. The results demonstrated that the method is suitable for the analysis of di- to deca-brominated diphenyl ethers and BB153 in the ambient air with precise quantification.