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1.
建立了生物介质内22种多溴联苯(PBBs)和27种多溴联苯醚(PBDEs)的净化和分析方法。通过分析不同时间段凝胶渗透色谱(GPC)洗脱液中49种化合物含量,得出不同化合物凝胶色谱洗脱曲线。样品经过凝胶渗透色谱-混合硅胶柱净化后,再使用GC-(NCI)/MS对样品进行检测。实验结果表明,PBBs和PBDEs检出限分别为0.02~0.88 pg/g和0.01~74.00 pg/g。对实验过程进行验证发现,样品不同浓度加标回收率为80%~120%,相对标准偏差小于20%。该方法具有良好的净化效果、准确度和精密度,拥有良好的线性范围及检出限,满足生物介质中溴代阻燃剂的检测分析实际要求。  相似文献   

2.
分析了辽宁省4个典型城市淡水鱼类中多溴联苯醚(PBDEs)和六溴环十二烷(HBCDs)的富集特征,并进行了健康风险评估。结果表明:淡水鱼类体内PBDEs和HBCDs检出率均为100%,PBDEs和HBCDs的平均质量分数分别为9.73 和21.81 ng/g(脂重)。PBDEs中的单体BDE 183、BDE 209和BDE 153在辽河流域不同鱼类的同源种中占优势,分别占PBDEs的26.8%~40%,17%~44%和14%~22%。在HBCDs的3种同系物中,α-HBCD是主要的单体,其相对贡献率为45.15%~84.71%。辽河流域的工厂企业生产活动对淡水鱼类产生了影响,居民通过消费水产品摄入PBDEs和HBCDs。健康风险评估结果显示:PBDEs和HBCDs的健康风险指数均<1,说明当地水产品中PBDEs和HBCDs的非致癌风险处于可接受水平。  相似文献   

3.
建立了土壤和沉积物中8种多溴联苯醚(PBDEs,BDE-28、BDE-47、BDE-99、BDE-100、BDE-153、BDE-154、BDE-183和BDE-209)加速溶剂同时萃取和净化-气相色谱-三重四极杆串联质谱(ASE-GC-MS-MS)的分析方法。通过优化加速溶剂萃取与弗罗里硅土在线净化和串联质谱多反应监测模式的条件,较好地去除基质干扰,并提高了三重四极杆串联质谱定性的准确性及定量的灵敏性。该方法采用改进的色谱柱能同时分析包括高溴代联苯醚BDE-209在内的8种PBDEs,其浓度范围为1~100 ng/mL(BDE-209为10~1 000 ng/mL),线性良好,线性回归系数均大于0.997。方法检出限为0.004~0.1 ng/g,方法回收率为75%~110%,方法精密度为2.4%~15.6%。适于批量处理土壤和沉积物中含有多组分痕量PBDEs的样品。  相似文献   

4.
为了解多溴联苯醚(PBDEs)和有机磷阻燃剂(OPFRs)在太湖3条主要入湖河流(太滆运河、太滆南运河和漕桥河)中的污染现状,采集其水体和沉积物样品,利用GC-MS/MS和LC-MS/MS技术对介质中13种PBDEs同族体和9种OPFRs进行分析。结果表明,所有水样品中均检出OPFRs,其总质量浓度为165~504 ng/L,其中三(1-氯-2丙基)磷酸酯(TCPP)为最主要污染物,最高值为160 ng/L;PBDEs在所有沉积物样品中均有检出,总质量比为16.7~765 ng/g。沉积物中PBDEs和OPFRs存在显著的正相关性(p<0.01),说明这2种化合物的污染来源和环境归趋可能相类似。水中OPFRs基于无效应浓度(PNEC)的风险评价显示,部分化合物对藻类、蚤类和鱼类具有中等生态风险。指出,随着PBDEs的禁用,以及潜在的生物累积效应,OPFRs的环境污染须引起进一步的关注。  相似文献   

5.
在总结药品及个人护理品(PPCPs)在水环境中分布特征的基础上,分析和对比了典型PPCPs在不同营养级水生生物(浮游植物、底栖生物和鱼类)体内的累积规律,并阐述了PPCPs在鱼体内的代谢转化途径和机理.提出未来该领域的主要研究方向包括加强对个人护理品生物累积和食物链传递的研究,深入探索PPCPs在食物链上的传递和累积规律,开展实际水体中PPCPs的代谢转化研究.  相似文献   

6.
采用分流进样模式,以GC-NCI-MS法测定土壤样品中7种高溴代联苯醚,对比了分流、不分流2种进样模式下的灵敏度、峰形、回收率、检出限。结果表明,在分流进样模式下,高溴代联苯醚在进样口的热分解率大大降低,色谱峰形尖锐无拖尾,测定结果线性范围宽,7种高溴代联苯醚的基质加标回收率为83.25%~94.71%,RSD为2.91%~7.37%,检出限为0.26~2.71 ng/g,与不分流进样模式相比,该方法灵敏度、检出限更高,适用于环境样品中高溴代联苯醚的检测分析。  相似文献   

7.
建立了一种超高效液相色谱串联质谱法(UPLC-MS/MS)同时测定土壤中8种多溴联苯醚化合物(PBDEs)的方法,采用快速溶剂萃取(ASE)和凝胶净化色谱(GPC),经BEH反相C18色谱柱分离,10 min内完成分离,使用含0.1%氨水的甲醇和水进行梯度洗脱,采用液相色谱-负离子-大气压化学电离(APCI)串联质谱,多反应监测模式(MRM),加入 13C12-BDE-139和13C12-BDE-209内标作定量分析。结果表明:在优化的分析条件下,PBDEs的线性相关系数为0.998 8~0.999 5,方法检出限为0.22~0.59 μg/kg,在2个添加水平下,平均回收率为71%~126%,标准偏差为3%~18%,土壤实际质控样测定结果均在允许范围内。适合于土壤中PBDEs的快速分析,特别对于高溴代PBDEs,相比气相色谱质谱方法具有更快的分析速度和更好的稳定性。  相似文献   

8.
分别采用微波萃取-气相色谱/质谱法、加速溶剂萃取提取-液相色谱/质谱法对采自太滆运河5个沉积物样品中的6种邻苯二甲酸酯类(PAEs)、13种多溴联苯醚(PBDEs)和9种有机磷酸酯(OPEs)的质量比及分布进行研究。结果表明,所有样品中均检测到PAEs、PBDEs和OPEs(以总量计),其总质量比分别为1.99~6.90μg/g,47~572和17.1~69.7 ng/g;十溴联苯醚(BDE-209)和磷酸三异辛酯(TEHP)分别是质量比最高的PBDEs和OPEs;对于PAEs,入太湖点位处邻苯二甲酸二(2-乙基己基)酯(DEHP)质量比较高,其余点位则是邻苯二甲酸二正丁酯(DBP)质量比较高;ω(PAEs)、ω(PBDEs)和ω(OPEs)两两间线性相关性较好,指示其来源相同;下游沉积物中污染物的质量比均高于上游,沿岸生产、生活中增塑剂和阻燃剂对太湖的污染应引起更多关注。  相似文献   

9.
采用快速溶剂萃取-固相萃取-液相色谱串联质谱法(LC-MS/MS)测定土壤中8种多溴联苯醚类(PBDEs)化合物,通过优化试验条件,使方法在100 μg/L~1 000 μg/L范围内线性良好,方法检出限为085 μg/kg~125 μg/kg。不同土壤样品的8种多溴联苯醚回收率为68.6%~127%,4次测定结果的RSD为4.8%~27.6%。将该方法用于测定电子废物拆解点周边的土壤样品,结果BDE-209测定值为未检出~168 μg/kg,BDE-183为未检出~560 μg/kg,其余6种BDEs均为未检出。  相似文献   

10.
以多溴联苯醚典型单体2,2′,4,4′?四溴联苯醚(BDE?47)为研究对象,阐明了其在土壤矿物质与有机质上的吸附解吸行为及特征。结果表明:土壤中无机矿物质对BDE?47的吸附贡献不大,而有机质是调控BDE?47在土壤中吸附行为的关键组分;有机质对BDE?47的吸附能力与其有机碳含量和物理化学特性相关;BDE?47在腐殖酸上的解吸存在显著的滞后现象。  相似文献   

11.
The occurrence of selected brominated flame retardants, including nine polybrominated diphenyl ether (PBDE) congeners, hexabromocyclododecane (HBCDD) and tetrabromobisphenol A (TBBPA) in leachate samples from eight landfill sites in South Africa, were investigated. In addition, the possible influences of dissolved organic carbon on their levels were also evaluated. Filtered leachate samples were subjected to solid-phase extraction to isolate the various target compounds. PBDEs with six bromine substituents and above, as well as α-HBCDD, β-HBCDD and TBBPA, were generally found below the detection limit. However, the mean value of the total lower PBDE congeners ranged between 0.04 and 0.48 μg L?1, and the concentrations of γ-HBCDD ranged from not detectable (ND) to 0.05 μg L?1. No significant correlation was observed between the target compounds and dissolved organic carbon, although weak to moderate correlations were mostly observed for the lower PBDEs.  相似文献   

12.
The environmentally prevalent polybrominated diphenyl ether (PBDE) #47 and polychlorinated biphenyls (PCBs) #28 and #118 were challenged for 24 hours with a novel biomass-supported Pd catalyst (Bio-Pd(0)). Analysis of the products via GC-MS revealed the Bio-Pd(0) to cause the challenged compounds to undergo stepwise dehalogenation with preferential loss of the least sterically hindered halogen atom. A mass balance for PCB #28 showed that it is degraded to three dichlorobiphenyls (33.9%), two monochlorobiphenyls (12%), and biphenyl (30.7%). The remaining mass was starting material. In contrast, while PCB #118 underwent degradation to yield five tetra- and five trichlorinated biphenyls, no less chlorinated products or biphenyl were detected, and the total mass of degraded products was 0.3%. Although the Bio-Pd(0) material was developed for treatment of PCBs, a mass balance for PBDE #47 showed that the biocatalyst could prove a potentially useful method for treatment of PBDEs. Specifically, 10% of PBDE #47 was converted to identifiable lower brominated congeners, predominantly the tribrominated PBDE #17 and the dibrominated PBDE #4, 75% remained intact, while 15% of the starting mass was unaccounted for.  相似文献   

13.
In this paper, we summarize spatial and temporal trends of polybrominated diphenyl ethers (PBDEs) and hexabromocyclododecanes (HBCDs) in coastal and marine biota, and further assess human exposure to these brominated flame retardants (BFRs) in Asia-Pacific. The review is based mainly on the studies that were conducted in our laboratory and utilized samples archived in the environmental specimen bank (es-BANK) of Ehime University, Japan. The studies suggest that the target BFRs are ubiquitous in the environment of Asia-Pacific. Examination of spatial trends reveals that concentrations of these contaminants are relatively high in samples from Korea, South China and Japan. In general, the magnitude of environmental contamination by PBDEs in Asia-Pacific, as well as human exposure to these contaminants, seem to be comparable to or slightly higher than in Europe, but lower than in North America. Evaluation of temporal trends in concentrations of BFRs in marine mammals from the coastal waters of Japan and China showed drastic increase during the last 30 years. These changes in BFR levels in samples from Japan were in line with trends in production/use of the commercial formulations. Since the withdrawal of some PBDE products from the Japanese market in the 1990s, concentrations of HBCDs appear to exceed those of PBDEs, reflecting increasing usage of HBCDs over PBDEs. The increasing environmental contamination by BFRs in Chinese coastal waters indicates that contamination by BFRs has already become evident, even in developing countries. In view of the rising environmental levels and the high consumption volume of BFRs in Asia, further efforts should be made to monitor environmental contamination by these chemicals in order to identify sources and reduce emissions.  相似文献   

14.
62 riverine and marine sediments were collected from the Laizhou Bay area, where the largest manufacturing base of brominated flame retardants (BFRs) in Asia is located. Eight polybrominated diphenyl ethers (PBDEs) were analyzed to investigate the impact of rapidly-developed bromine industries on the regional aquatic system. PBDE concentrations varied largely in riverine sediments. Σ(7)PBDEs (including BDE 28, 47, 99, 100, 153, 154 and 183) and BDE 209 ranged from 0.01 to 53 ng g(-1) dw and from 0.74 to 285 ng g(-1) dw with a mean value of 4.5 ng g(-1) dw and 54 ng g(-1) dw, respectively, indicating a strong influence of direct pollution discharges from local factories. In marine sediments, Σ(7)PBDEs and BDE 209 ranged from not detected (nd) to 0.66 ng g(-1) dw and from 0.66 to 12 ng g(-1) dw with a mean value of 0.32 ng g(-1) dw and 5.1 ng g(-1) dw, respectively. PBDE concentrations were mostly <10 ng g(-1) dw for Σ(7)PBDEs and <50 ng g(-1) dw for BDE 209, which are at a relatively low level for monitored riverine and coastal sediments around the world. Even at the most contaminated sites in Laizhou Bay area, PBDE concentrations were not among the highest concentrations reported in the literature. Congener compositions were dominated by BDE 209 (57.2-99.9% of the sum of BDE congeners), with minor contributions from penta- and octa-BDE products. Tri- to octa-BDE congeners were well correlated among each other (r > 0.75) and thus sources from similar mixing of penta- and octa-BDE products were suggested in this area. Compared with riverine sediments, a much better correlation between PBDE concentrations with TOC was observed in marine environment. The congener pattern changed and their correlation coefficients among each other were remarkably reduced. Contributions of BDE 28, 47 and 99 to Σ(7)PBDEs were generally the same in almost all the marine sites, while it was distinctively higher for BDE 153. These are probably attributable to several reasons, such as contributions by atmospheric deposition and/or redistribution between particles of various sizes during and/or after fluvial transportation combined with the difference of physiochemical properties of BDE congeners.  相似文献   

15.
Brominated flame retardants (BFRs) have been used extensively and are considered ubiquitous contaminants. To evaluate exposure to brominated flame retardants within an electronic recycling facility personal air monitoring was done during a two year period. A total of 22 polybrominated diphenyl ethers (PBDEs) and 2 other bromine containing organic compounds have been analysed and evaluated in 17 personal air samples. The most abundant congeners of PBDE was #209 (<0.7-61 ng m(-3)), #183 (<0.1-32 ng m(-3)) indicating the use of the commercial octaBDE mixture, followed by PBDE #99 and #47 (<1.3-25 and <0.9-16 ng m(-3), respectively). The second most abundant peak in the chromatogram from all samples was identified as 1,2-bis(2,4,6-tribromophenyxy)ethane (BTBPE) in the concentration range <0.6-39 ng m(-3) (semi-quantitatively calculated against PBDE #191). A second bromine containing compound was also detected, structurally similar to decabromodiphenyl ethane (DeBDethane), however no definite identification could be made. The air samples were also evaluated on a work exposure category basis. The workers represented three different categories: dismantlers, other workers and unexposed. There was a significant difference (p < 0.05 with the Mann-Whitney test) among the dismantlers and the unexposed categories for PBDE congeners #47, #100, #99, #154; #153, #183, #209 and BTBPE. Another observation was that the air concentrations of PBDEs and BTBPE in the breathing zone were negatively correlated (p < 0.05) to the amount of recycled material (in kg). The present work shows that the exposure to brominated flame retardants varied within the electronic facility and that further research is needed to evaluate how the exposure differs with different products being dismantled as well as how the bioavailability of the different BFRs to humans is related to particle exposure.  相似文献   

16.
Polybrominated diphenyl ethers (PBDEs) have been reported in air, surface waters, suspended sediments, soil, sediment, fish, marine mammals, and bird eggs throughout Canada, from the St. Lawrence Estuary to the Strait of Georgia and the northernmost reaches of the Canadian Arctic. Canadian scientists have detected the presence of PBDEs in breast milk in every Canadian province. In fact, recent data on temporal trends strongly suggests that the concentrations of PBDEs are on the rise in the Canadian environment. These findings are similar to those reported in other nordic countries, and have prompted several countries to implement environmental monitoring programs. Among the key challenges currently facing Canada and other countries concerns how best to measure these chemicals in different matrices. In this paper, several analytical methods cited in the scientific literature for determining PBDE concentrations in different abiotic and biological matrices are reviewed. The critical criteria required for accurate determination of PBDEs in complex environmental matrices are discussed, including instrument sensitivity, reliability, potential interference's and the need for specialized instrumentation for the determination of compounds up to 975 Daltons. While a single analytical method that meets these and other criteria has not yet been perfected by scientists, GC/HRMS-based methods amenable to isotope dilution techniques warrant further refinement, and likely represent the best tools for future environmental monitoring programs.  相似文献   

17.
The reduction in the use of polybrominated diphenyl ethers (PBDEs) and hexabromocyclododecane (HBCD) has opened the way for the introduction of novel brominated flame retardants (NBFRs) in place of the banned formulations. Important representatives of this group are decabromodiphenyl ethane (DBDPE), 1,2-bis(2,4,6-tribromophenoxy) ethane (BTBPE), hexabromobenzene (HBB), and pentabromoethylbenzene (PBEB). In this study, the contamination due to NBRFs was investigated for the first time in Italy in the sediments of Lake Maggiore. The aim of the research was to characterize in detail the possible presence of temporal trends and/or to identify potential sources of contamination. The study also considered the PBDE and HBCD lake sediment’s current contamination. The analytical results showed that sediments in Lake Maggiore and its tributary rivers had weak concentrations of PBEB, HBB, and BTBPE, but they did not have a negligible/insignificant contamination of HBCD (up to 23.7 ng/g dry weight (d.w.)). The determination of PBDEs in sediments showed that BDE-209 was the predominant congener (up to 217 and 28 ng/g d.w. in river and lake sediments, respectively). DBDPE was detected in the sediments with relevant concentrations (up to 280 ng/g d.w in the River Boesio sediments). The positive correlation of DBDPE with BDE-209 confirmed the wide and important use of this compound in the Lake Maggiore basin and the hypothesis that this compound will soon become one of the most important NBFRs used in Northern Italy. The contamination of Lake Maggiore sediments due to PBDEs, HBCD, and NBFRs were comparable to other worldwide situations.  相似文献   

18.
The concentrations and distributions of some typical chlorinated flame retardants (Dechlorane or Mirex, Dechlorane 602 (Dec 602), Dechlorane 603 (Dec 603), Dechlorane 604 (Dec 604) and Dechlorane Plus (DP)) and brominated FRs (polybrominated diphenyl ethers (PBDEs), pentabromoethylbenzene (PBEB) and 1,2-bis(2,4,6-tribromophenoxy)ethane (BTBPE)) were analyzed in surficial sediment collected from the Dalian coastal area in northeast China. Dec 603, Dec 604, and BTBPE were below their respective limits of detection (LOD) in all sediment samples, while Dechlorane, Dec 602, DP, Σ13BDE (tri- to hepta-BDEs), BDE 209, and PBEB were identified in the ranges <0.015-39.9 ng g(-1) dry weight (dw), <0.011-0.156 ng g(-1) dw, 0.69-7.00 ng g(-1) dw, 0.017-1.33 ng g(-1) dw, 3.94-103 ng g(-1) dw, and <0.073-1.9 ng g(-1) dw, respectively. Relationships between these chlorinated and brominated FRs were analyzed using Pearson's correlation and principal component analysis (PCA). DP, Dechlorane, Σ13BDE, and BDE 209 showed significantly positive correlation (p<0.05), and these relationships showed excellent agreement with PCA results. The spatial trends for Dechlorane, DP, BDE 209, and Σ13BDE showed that high concentrations were found in the industrial zone and lower concentrations in residential and garden zones. The results imply that these FRs are originating from a common source, and support the view that direct input from the effluent of sewage outlets is a major source of these compounds in Dalian sediment.  相似文献   

19.
This paper presents preliminary data on polybrominated diphenyl ethers (PBDEs) in the Scottish aquatic environment. Sediment and biota (fish liver, fish muscle and mussels) from a number of locations around Scotland were analysed for PBDEs with samples being from both remote and from potentially contaminated areas such as the former sewage sludge dump site at Garroch Head in the Clyde. PBDEs were measured in both cultivated, rope grown mussels and wild mussels collected from 5 sites around Scotland in 2006. Total PBDE concentrations (sum of tri- to hepta-BDEs) ranged from 相似文献   

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