加速溶剂萃取-同步净化／气相色谱-质谱法检测沉积物中4种新型溴代阻燃剂
文献类型：期刊论文
| 作者 | 裴镜澄; 吴明红; 向甲甲; 彭兵权; 徐刚; 孙延枫; 顾建忠; 雷建求 |
| 刊名 | 分析测试学报
 |
| 出版日期 | 2014 |
| 卷号 | 33期号:7页码:773 |
| 关键词 | 加速溶剂萃取 固相萃取 气相色谱-质谱法 沉积物 溴代阻燃剂 |
| 其他题名 | Determination of Four Kinds of Novel Brominated Flame Retardants in Sediments by Gas Chromatography - Mass Spectrometry Combined with Accelerated Solvent Extraction - Synchronous Purification |
| 中文摘要 | 建立了同时测定沉积物中2-乙基己基-四溴苯甲酸(TBB)、1， 2-二（2， 4，6-三溴苯氧基）乙烷(BTB-PE)、2,3,4,5-四溴-苯二羧酸双（2-乙基己基）酯(TBPH)及十溴二苯乙烷(DBDPE) 4种新型溴代阻燃剂的加速溶剂萃取-同步净化/气相色谱-质谱分析方法。冷冻干燥后的环境沉积物样品经改进后的加速溶剂萃取(ASE)并净化后，浓缩液过Florisil固相萃取小柱，用4 mL正己烷和二氯甲烷分步洗脱，氮吹定容后用气相色谱-质谱(GC-MS)检测。结果表明，4种溴代阻燃剂的线性范围为2~1 000mug·L~(-1)（其中DBDPE为20?10000mug? L~(-1)），相关系数均大于0.995，定量下限(S/N≥10)为0.074 ~ 44.4mug? kg~(-1)；在2，10mug? L ~(-1)两个加标水平下的方法回收率为79. 5% ~ 119. 7% ，相对标准偏差为2. 6%~ 15. 3%。采用本方法对上海市主要水体中6个河流段采样点沉积物中的4种新型溴代阻燃剂进行检测，除1个采样点未检出TBB外，其余采样点均检出4种新型溴代阻燃剂。该方法简便、快速、灵敏度高、定性定量准确，满足沉积物中新型溴代阻燃剂的检测要求。 |
| 英文摘要 | A simple method based on accelerated solvent extraction ( ASE) /solid phase extraction (SPE) coupled with gas chromatography - mass spectrometry( GC - MS) was developed for the simultaneous determination of 2-ethylhexyl-2, 3,4,5-tetrabromobenzoate ( TBB ), 1,2-bis ( 2, 4,6tribromophenoxy ) ethane ( BTBPE ),bis ( 2-ethylhexyl) 2, 3,4, 5-tetrabromophthalate ( TBPH ) and decabromodiphenylethane( DBDPE ) in sediments. Extraction and cleanup of four novel brominated flame retardants in lyophilized sediments were performed by improved accelerated solvent extraction (ASE),and the concentrated solution was cleanup using Florisil solid phase extraction cartridges with 4 mL hexane,then eluted with 4 mL dichloromethane. The eluents was concentrated under a gentle N2 stream and analyzed by GC - MS. The calibration curves were linear in the range of 20 10 000 mug ? L~(-1) for DBDPE, and 2-1 000 mug · L~(-1) for the rest of compounds， with correlation coefficients more than 0. 995. The instrumental limits of quantitation ( S/N ≥ 10 ) for target compounds were in the range of 0. 074 - 44. 4 mug ? kg~(-1). The average recoveries of target compounds at two spiked levels(2, 10 mug ? L~(-1) ) were in the range of 79. 5% - 119. 7%,with relative standard deviations( RSDs) of 2. 6% - 15. 3% . The proposed method was applied in the determination of four novel brominated flame retardants in sediments at six different sediments sampling sites from principal watersheds of Shanghai. All samples were detected to be contain TBB, BTBPE, TBPH and DBDPE, except one sampling site without TBB. The method was simple and sensitive, and could meet the requirements for rapid and accurate determination of four novel brominated flame retardants. |
| 收录类别 | CSCD |
| 语种 | 中文 |
| CSCD记录号 | CSCD:5201195 |
| 版本 | 出版稿 |
| 源URL | [http://ir.siom.ac.cn/handle/181231/12927]  |
| 专题 | 上海光学精密机械研究所_空间激光信息技术研究中心 |
| 作者单位 | 1.裴镜澄, 上海大学环境与化学工程学院, 上海 200444, 中国. 2.吴明红, 上海大学环境与化学工程学院, 上海 200444, 中国. 3.向甲甲, 上海大学环境与化学工程学院, 上海 200444, 中国. 4.彭兵权, 上海大学环境与化学工程学院, 上海 200444, 中国. 5.徐刚, 上海大学环境与化学工程学院, 上海 200444, 中国. 6.孙延枫, 上海大学环境与化学工程学院, 上海 200444, 中国. 7.顾建忠, 上海大学环境与化学工程学院, 上海 200444, 中国. 8.雷建求, |
| 推荐引用方式 GB/T 7714 | 裴镜澄,吴明红,向甲甲,等. 加速溶剂萃取-同步净化／气相色谱-质谱法检测沉积物中4种新型溴代阻燃剂[J]. 分析测试学报,2014,33(7):773. |
| APA | 裴镜澄.,吴明红.,向甲甲.,彭兵权.,徐刚.,...&雷建求.(2014).加速溶剂萃取-同步净化／气相色谱-质谱法检测沉积物中4种新型溴代阻燃剂.分析测试学报,33(7),773. |
| MLA | 裴镜澄,et al."加速溶剂萃取-同步净化／气相色谱-质谱法检测沉积物中4种新型溴代阻燃剂".分析测试学报 33.7(2014):773. |
入库方式： OAI收割
来源：上海光学精密机械研究所
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