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1.
高分辨质谱法测定海鱼中二噁(口英)和多氯联苯   总被引:1,自引:0,他引:1  
目的采用同位素稀释的HRGC/HRMS法定量检测鱼体中17种2,3,7,8-氯取代的二噁(口英)(PCDD/Fs)和12种二噁(口英)多氯联苯(PCBs).方法参照美国EPA1613及EPA1668A方法,采用索式抽提和自动纯化系统(FMS)对鱼体中的PCDD/Fs及PCBs进行纯化和富集、用同位素稀释气相色谱与高分辨质谱联用-多离子检测方法检测.结果该方法可对样品中的PCDD/Fs及PCBs同系物进行有效分离,PCDD/Fs同位素标准物的回收率为83.83%~98.48%,PCBs同位素标准物的回收率为50.06%~90.56%.13种PCDD/Fs在鱼体中可检出,总毒性当量(TEQ)为0.86 pg/g,12种二噁(口英)PCBs在鱼体中均可检测出,总TEQ值为2.77pg/g.结论该方法可以同时对同一样品中的17种PCDD/Fs及12种二噁(口英)PCBs进行检测,检测效率高,结果准确可靠.  相似文献   

2.
高分辨质谱法测定海鱼中二噁英和多氯联苯   总被引:3,自引:0,他引:3  
目的采用同位素稀释的HRGC/HRMS法定量检测鱼体中17种2,3,7,8-氯取代的二噁英(PCDD/R)和12种二噁英多氯联苯(PCBs)。方法参照美国EPA1613及EPA1668A方法,采用索式抽提和自动纯化系统(FMS)对鱼体中的PCDD/Fs及PCBs进行纯化和富集、用同位素稀释气相色谱与高分辨质谱联用一多离子检测方法检测。结果该方法可对样品中的PCDD/Fs及PCBs同系物进行有效分离,PCDD/Fs同位索标准物的回收率为83.83%~98.48%,PCBs同位素标准物的回收率为50.06%~90.56%。13种PCDD/Fs在鱼体中可检出,总毒性当量(TEQ)为0.86pg/g,12种二噁英PCBs在鱼体中均可检测出,总TEQ值为2.77pg/g。结论该方法可以同时对同一样品中的17种PCDD/Fs及12种二噁英PCBs进行检测,检测效率高,结果准确可靠。  相似文献   

3.
〔目的〕采用高分辨气相色谱 高分辨双聚焦磁式质谱联用仪 (HRGC HRMS)定量检测了鱼体中 12种类二口恶英多氯联苯 (PCBs)化合物。〔方法〕参照美国EPA1668A方法 ,采用索式抽提和自动纯化系统 (FMS)等仪器对鱼体样品中的类二口恶英PCBs进行纯化和富集、用同位素稀释气相色谱与高分辨质谱联用 -多离子检测方法检测。〔结果〕该方法可对PCBs同系物进行有效分离 ,同位素标准物的回收率分布于 44 .8%~ 93 .1%之间 ,CSL考核样的检测结果均在令人满意的范围之内 ,7种类二口恶英PCBs在鱼体中可检测出 ,总TEQ值为 0 .3 5pg g。〔结论〕该方法可以准确检测样品中类二口恶英PCBs ,所检鱼体中含有一定量类二口恶英PCBs ,有必要做更多样品 ,对其污染情况做出评价。  相似文献   

4.
海水鱼体中的二(口恶)英类化合物分析   总被引:1,自引:0,他引:1  
目的对海水鱼体内二(口恶)英检测方法的研究.方法参照美国EPA1613方法,采用索式抽提和自动纯化系统等仪器对鱼体中的二(口恶)英组分进行纯化和富集、用同位素稀释气相色谱与高分辨质谱联用-多离子检测方法检测.结果该方法的检测限为0.001 pg/g~0.176 pg/g,仪器检测限为6.5fg~157.9fg,同位素标准物的回收率分布于70.81%~87.33%之间,17种2,3,7,8-氯取代的二(口恶)英类化合物在鱼体中均可检测出,总TEQ值为1.117 pg/g.结论本实验室方法可以准确检测样品中二(口恶)英类化合物,所检鱼体中含有二(口恶)英化合物,有必要做更多样品,对其污染情况做出评价.  相似文献   

5.
目的 建立人体胎盘组织样品氯化二苯并二噁英(PCDD)和呋喃(PCDFs)、多氯联苯(PCBs)、多溴联苯醚(PBDEs)化合物同时准确定量检测分析方法,揭示上述持久性有机污染物人体负荷水平,并初步进行危险性评估.方法 采用国际权威标准方法--核素(同位素)稀释的高分辨气相色谱/高分辨双聚焦磁式质谱联用(HRGC/HRMS)技术,以多离子检测方法对人体胎盘组织样品中17个PCDD/Fs和12个共平面PCBs以及7个PBDEs化合物分别进行定性和定量分析,用WHO-TEF值计算所有样品的毒性当量浓度∑TEQ(PCDD+PCDFs+PCBs)和PBDEs浓度,进一步对人体二嗯英和PBDEs化合物负荷水平进行危险性评估.结果 6个胎盘组织样品中PCDD/Fs和PCBs化合物毒性当量总浓度∑TEQ(PCDD+PCDFs+PCBs)中位数是18.15 WHO-TEQ pg/g脂肪.范围分布在5.14~67.01 WHO-TEQ pg/g脂肪之间.2,3,4,7,8-PeCDFs、1,2,3,7,8-PeCDDs、PCB126是毒性当量的主要贡献者,合计占65%.以7个化合物计算PBDEs总浓度,6个样品的中位数值为2.73 ng/g脂肪,均数为7.17 ng/g脂肪,范围是0.95~25.99 ng/g脂肪.BDE47是最主要的污染同系物,占到35%.浓度最高的一个受试样品其毒性当量总浓度∑TEQ(PCDD+PCDFs+PCBs)已经达到世界上已知高暴露区人体二噁英污染负荷水平.结论 我们在本研究中建立了人体组织样品中持久性有机化合物二噁英和PBDEs化合物同时准确定量检测方法,高二噁英负荷水平的样品提供者可能对胎儿存在健康危害的高暴露风险,对于健康的远期影响还需要深入进行医学追踪研究.  相似文献   

6.
目的 了解某市市售牛奶及其制品中二噁英类化合物污染情况.方法 于2007年2-6月采集某市市售液体牛奶和奶粉(各5份),用高分辨气相色谱.高分辨双聚焦磁式质谱联用仪(HRGC-HRMS)定量检测样品中的二噁英及多氯联苯水平.采用索式抽提装置、FMS自动纯化系统对市售液体牛奶及奶粉样品中的二噁英(PCDD/Fs)及多氯联苯(PCBs)组分进行纯化和富集,采用同位素稀释法,以HRGC/HRMS联用仪检测.结果 奶粉和液体牛奶的总TEQ[∑(PCDD/Fs+PCBs)]平均值分别是0.43Pg/g脂肪和3.83ps/g脂肪,中位数分别是0.34Pg/g脂肪和2.04pgg脂肪.所有奶样的总TEQ[∑(PCDD/Fs+PCBs)]均值是2.13 ps/g脂肪,中位数是0.815 pg/g脂肪.本次调查的所有样品的平均总TEQ[∑(PCDD/Fs+PCBs)]远低于欧盟所设定的奶品二噁英类化合物的限量标准.受试样品中除了两种液体牛奶样品二噁英类化合物总TEQ超过欧盟限量标准外,其他液体牛奶和奶粉样品二噁英及多氯联苯含量远低于欧盟的限量标准.但是,液体牛奶的平均二噁英浓度明显高于奶粉样品.结论 本次采集的市售牛奶及其制品存在二噁英类化合物的污染.  相似文献   

7.
目的了解某市市售牛奶及其制品中二[口][恶]英类化合物污染情况。方法于2007年2-6月采集某市市售液体牛奶和奶粉(各5份),用高分辨气相色谱-高分辨双聚焦磁式质谱联用仪(HRGC-HRMS)定量检测样品中的二[口][恶]英及多氯联苯水平。采用索式抽提装置、FMS自动纯化系统对市售液体牛奶及奶粉样品中的二[口][恶]英(PCDD/Fs)及多氯联苯(PCBs)组分进行纯化和富集,采用同位素稀释法,以HRGC/HRMS联用仪检测。结果奶粉和液体牛奶的总TEQ[∑(PCDD/Fs+PCBs)]平均值分别是0.43pg/g脂肪和3.83pg/g脂肪,中位数分别是0.34pg/g脂肪和2.04pg/g脂防。所有奶样的总TEQ[∑(PCDD/Fs+PCBs)]均值是2.13pg/g脂肪,中位数是0.815pg/g脂肪。本次调查的所有样品的平均总TEQ[∑(PCDD/Fs+PCBs)]远低于欧盟所设定的奶品二[口][恶]英类化合物的限量标准。受试样品中除了两种液体牛奶样品二[口][恶]英类化合物总TEQ超过欧盟限量标准外,其他液体牛奶和奶粉样品二嗯[口][恶]英及多氯联苯含量远低于欧盟的限量标准。但足,液体牛奶的平均二[口][恶]英浓度明显高于奶粉样品,结论本次采集的市售牛奶及其制品存在二[口][恶]英类化合物的污染。  相似文献   

8.
目的:检测分析市售鱼体中PCDD/Fs,PCBs和PBDEs的污染水平。方法:采集市售16种鱼样品,通过索氏抽提,酸性硅胶处理,利用硅胶柱和铝柱净化,分离开PCDD/Fs,PCBs和PBDEs,用高分辨气相色谱/高分辨质谱检测分析PCDD/Fs,PCBs和PBDEs。结果:鱼样品中PCDDs/PCDFs的毒性当量值为0.024pgWHO-TEQ/g.ww~0.31 pgWHO-TEQ/g.ww之间,PCBs的毒性当量值为0.04 pgWHO-TEQ/g.ww~1.50 pgWHO-TEQ/g.ww之间,12种Co-PCBs和7种指示性PCBs相加的总PCBs含量为92.57 pg/g.ww~10893.60 pg/g.ww之间,PBDEs含量在50.38 pg/g.ww~1622.86 pg/g.ww之间。结论:鱼体中PCDDs/PCDFs、PCBs和PBDEs污染的相关性比较高,三者有着相同的污染途径。鱼体中PCDD/Fs,PCBs和PBDEs的污染处于相对安全的水平,但持久性有机污染物对环境污染引起的食品污染问题应该引起重视。  相似文献   

9.
2007年北京市居民母乳中二噁英类化合物负荷水平调查   总被引:1,自引:0,他引:1  
目的 调查北京地区居民母乳中多氯代苯并二噁英和多氯代苯并呋喃(PCDD/Fs)和二噁英样多氯联苯(dl-PCBs)的污染水平,评价一般人群PCDD/Fs和dl-PCBs的机体负荷状况.方法 2007年在北京市11个区、县中采集母乳样品110份,制成11个混合样品后,采用同位素稀释技术以高分辨气相色谱-高分辨质谱(HRGC-HRMS)测定母乳样品中的PCDD/Fs和dl-PCBs.结果 北京市母乳样品中二噁英类化合物含量最高的组分为八氯代二苯并二噁英(OCDD)和多氯联苯(PCB)-118、PCB-105,其含量中位数分别为20.6 pg/g脂肪、4.07和1.63 ng/g脂肪.按毒性当量(TEQ)计,北京市11个母乳混合样品中总二噁英类化合物含量中位数为7.4 pg TEQ/g脂肪;最高的为通州区,含量中位数为13.5 pg TEQ/g脂肪;最低的为平谷区,为4.3 pg TEQ/g脂肪.结论 目前北京市母乳中PCDD/Fs和dl-PCBs处于较低水平,但随着我国的快速工业化,人群此类物质的机体负荷水平有可能会上升,因此有必要持续跟踪监测.  相似文献   

10.
目的 评价典型行业所在地区食品样品中17种PCDD/Fs的污染水平.方法 使用同位素稀释技术以高分辨气相色谱-高分辨质谱(HRGC-HRMS)测定采自于垃圾焚烧厂、氯化工厂、铸造厂周边以及对照组地区的猪肉、牛肉、鸡肉、牛奶、鸡蛋、水产类及蔬菜样品中的17种二嗯英(PCDD/Fs).结果 OCDD是主要的污染物,平均含量值为0.75 pg/g wet weight;其次,垃圾焚烧厂、氯化工厂、铸造厂周边地区的食品样品中17种PCDD/Fs的毒性当量浓度(TEQ)会显著高于对照组,蔬菜样品中TEQ值会明显低于其他样品;另外,结合已有的食物消费量,计算标准人的二噁英类物质的每月膳食暴露量会远低于JECFA规定的PTMI(70 pg/kg bw/month).结论 垃圾焚烧厂,铸造厂和对照组周边地区人群目前由膳食摄入PCDD/F而导致的潜在健康风险处于较低的水平.  相似文献   

11.
我国某海域海鱼中二噁英污染分析   总被引:4,自引:0,他引:4  
目的对我国某海域20个海鱼样品进行了二噁英污染状况的定量分析检测,并对该地区人群从鱼获得的膳食暴露进行了初步评估。方法2003年6月至12月采集海水养殖鱼7类,20个样品。采用索式抽提装置、FMS专用净化装置对样品进行提取、纯化和富集,采用国际权威标准方法高分辨气相色谱/高分辨双聚焦磁式质谱联用(HRGC/HRMS)技术,以HRGC/HRMS多离子检测方式分析了样品中的17种氯化二苯并二噁英和氯化二苯并呋喃(PCDD和PCDF)化合物的含量,用放射性核素稀释技术定量。结果质控样品对方法的验证结果在国际认可的范围内,3次检测数据的相对标准偏差<15%。20个海鱼样品的总PCDD/PCDF平均含量以湿重计是1.48ng/kg,范围分布在0.21~8.10ng/kg湿重,以世界卫生组织毒性当量因子(WHOTEF)计,样品总毒性当量浓度(WHOTEQ)分布于0.030~1.291ng/kg湿重之间,平均总的毒性当量浓度是0.292ng/kg。以该TEQ值进行估算,该地区人群由鱼引起的二噁英污染暴露量估计为每日每公斤体重0.58pgWHOTEQ。结论不同样品间二噁英污染水平相差很大,人群由鱼引起的二噁英暴露量虽然低于世界卫生组织的标准,但若考虑人体多渠道摄入的食品,说明我国二噁英的污染现状不容忽视。  相似文献   

12.
Polychlorinated dibenzo-p-dioxins (PCDDs), dibenzofurans (PCDFs), and biphenyls (PCBs) were detected in sediments from Suzhou Creek with mean concentrations of 478.1, 245.1, and 4727.6 pg/g dw, respectively. WHO–TEQ concentrations of PCDD/Fs in sediments ranged from 2.90 to 13.96 pg/g dw, while TEQ concentrations of PCBs varied from 0.27 to 1.41 pg/g dw. OCDD or HpCDD were the dominant congeners but PeCDF or HpCDD was the major contributor to PCDD/Fs-TEQ in all the sites. For dioxinlike biphenyls, PCB 118 was the major congener while PCB-TEQ was attributable to PCB 126 in all the samples.  相似文献   

13.
Five bulked human adipose tissue samples were analyzed for individual polychlorinated biphenyl (PCB) congeners (including selected non-ortho-substituted compounds) and polychlorinated dibenzo-p-dioxins and furans (PCDD/Fs). Mean PCB and PCDD/F (tetra-through octachlorinated homologues) concentrations were 0.75 g/g and 1.22 ng/g adipose tissue respectively. Both the congener patterns and levels detected were similar to those reported by laboratories in other industrialised countries. Each sample comprised of tissue taken from donors within a given locality. However, no obvious relationships were apparent between sampling area, absolute concentrations and congener pattern of PCBs and PCDD/Fs.The contribution of individual PCDD/F and non -ortho-(o), mono-o-, and di-o-substituted PCB congeners to the total calculated toxic equivalent values (TEQ) was assessed for each sample. The main contributions to the TEQ were the mono-o-substituted PCB congeners #118 (TEQ=42.5 pg/g of lipid), #156 (TEQ=24.8 pg/g) and #105 (TEQ=20.7 pg/g), followed by 1,2,3,6,7,8-HxCDD (TEQ=18.2 pg/g), 2,3,4,7,8-P5CDF (TEQ= 12 pg/g), 1,2,3,7,8-P5CDD (TEQ=11.5 pg/g), and the non-o-substituted PCB congener #126 (TEQ =11.3 pg/g). Collectively, these compounds accounted for 80% of the STEQ values. Based on the TEFs proposed by Safe (1990), the overall TEQs calculated for the monitored PCBs, were twice those due to PCDD/Fs.  相似文献   

14.
High levels of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs), mono- and non-ortho-polychlorinated biphenyls (PCBs), and polybrominated dibenzo-p-dioxins (PBDDs) are found in fish from coastal areas in the Baltic Sea, which may cause ecotoxicological effects. To increase our understanding of the persistency of the emerging pollutants polybrominated dibenzo-p-dioxins and dibenzofurans (PBDD/Fs), fish feed was spiked with 21 PBDD/Fs, 17 PCDD/Fs, and 30 PCBs and fed to zebrafish (Danio rerio). Concentrations in fish and eggs were examined during a 6- or 12-week uptake period, and a 6-week elimination period. Steady-state was reached for 2-, 3-, 7-, and/or 8-substituted tri- and tetra-BDD/Fs; 2,3,7,8-tetra-BDD (2,3,7,8-TeBDD) was the most strongly retained. Steady-state was not reached for tetra- to hexa-CDDs. Non-2,3,7,8 congeners showed little or no retention. Most PCBs had high retention and did not reach steady state. Half-lives decreased in the order PCBs?>?PCDD/Fs?>?PBDD/Fs. Concentrations of 2,3,7,8-substituted penta- to octa-CDD/Fs decreased with their degree of chlorination, suggesting that the rate-limiting factor for uptake is low bioavailability. Maternal transfer was observed for all retained compounds, with most transfer factors <1, indicating that transfer rates are affected by the poor water solubility of the compounds. The limited retention of the major PBDD congeners found in Baltic Sea fish suggests that they are exposed to high or very high concentrations via either food or water.  相似文献   

15.
目的 了解深圳市城市饮用水中二噁英(PCDD/Fs)的污染水平和分布特征.方法 于2010年3-9月,采集深圳市5座自来水厂的原水和出厂水,参照美国环保局EPA23和EPA1613方法,采用同位素稀释的技术、通过高分辨气相色谱-高分辨双聚焦磁式质谱(HRGC/HRMS)仪对水样中17种具有毒性当量因子(TEF)的PCD...  相似文献   

16.
Adult Atlantic salmon (Salmo salar) were fed on four diets containing polychlorinated dibenzo-p-dioxins (PCDDs), polychlorinated dibenzofurans (PCDFs), and polychlorinated biphenyls (PCBs) for 30 weeks. Lipid-normalized concentrations showed that all congeners were equally partitioned between whole-fish and fillet samples. Skinned fillet accumulated approximately 30% of the total PCDD/F and PCB content in fish. Accumulation efficiencies in whole fish were 43% for 2,3,7,8-chlorinated dibenzo-p-dioxins and dibenzofurans, 83% for dioxin-like PCBs, and 78% for other PCB congeners. Among PCDD/Fs, tetra- and pentachlorinated congeners were preferentially accumulated in salmon, whereas hepta- and octachlorinated dibenzo-p-dioxins were excreted in the feces. Substitution patterns that were associated with a preferential accumulation of PCBs in salmon included non-ortho substitution and tetrachlorination. Accumulation efficiencies and lipid-normalized biomagnification factors (BMFs) were not influenced by the PCDD/F and PCB concentrations of the diets. Biomagnification (BMF > 1) of tetra- and pentachlorinated dibenzo-p-dioxins and dibenzofurans and of all the PCBs was observed. Differences in the behavior of PCDD/F and PCB congeners resulted in a selective enrichment of the most toxic congeners in salmon.  相似文献   

17.
We analyzed the weighted 2001-2002 National Health and Nutrition Examination Survey data to assess potential differences in mean total 2,3,7,8-tetrachlorodibenzo-p-dioxin (TCDD) TEQ between various groups of individuals and to determine serum reference concentrations for polychlorinated dibenzo-p-dioxins, dibenzofurans (PCDD/Fs) and dioxin-like polychlorinated biphenyls (PCBs) in the general US population. Differences appeared to exist between female smokers and non-smokers and between non-Hispanic groups and all other races. Potential differences were also observed among the four age groups with an increasing trend in mean total TCDD TEQ with increasing age. Both age and gender appeared to confound the association between smoking status and total TCDD TEQ, dictating the need for further analysis. As anticipated, PCBs contributed appreciably to the total TCDD TEQ levels in the referent population and accounted for 38% to 41% of the total TEQ depending on age. Nearly 80% of the mean total TCDD TEQ was attributable to four PCDD/F congeners and three PCB congeners. In this analysis, two methods were used to assess samples where the concentrations were below the limits of detection (LODs), and this did not have significant impact on the mean total TCDD TEQ at the higher percentiles and for older individuals. Comparison of our results to those from a recent PCDD/F biomonitoring study indicates that the mean TCDD TEQ serum concentration of the individuals studied does not appear to be different from typical levels found in the general US population. Additionally, an assessment of data from the National Human Adipose Tissue Survey using our referent statistics shows that levels of these chemicals have been declining in the general population for at least two decades. The reference TEQs presented in this paper provide relevant, current data that can be used to evaluate biomonitoring results of individuals or groups exposed or potentially exposed to PCDD/Fs and PCBs above referent levels.  相似文献   

18.
目的对中国某水域的海鱼和淡水鱼样品开展二英污染水平与同系物轮廓表征研究,并评估该典型地区人群通过鱼类暴露二英的膳食摄入量。方法通过布点抽样采集8个养殖点(海水与淡水各半)31份样品,以同位素稀释的HRGCHRMS-多离子检测方式测定样品中的PCDDsFs。结果海水养殖鱼和淡水养殖鱼中PCDDFs平均浓度以湿重计分别为1.43和3.34pgg,以WHOTEQ计分别为0.28pgg和0.43pgg。OCDD、2,3,7,8TCDF为最主要的优势污染同系物;如以毒性的主要贡献者计,则以1,2,3,7,8PeCDD、2,3,4,7,8PeCDF、2,3,7,8TCDD为主。该地区人群摄入鱼的二英PCDDFs的平均膳食暴露量的估算是0.63pgWHOTEQkgbw·day。结论该水域中的鱼已受到了一定程度的PCDDFs污染,淡水养殖鱼高于海水养殖鱼(约为1倍)。鱼体中所检测到的二英污染的平均水平低于欧盟制定的限量标准(3.0pgWHOTEQg)。  相似文献   

19.
Concentrations of polychlorinated dibenzo-p-dioxins (PCDDs), polychlorinated dibenzofurans (PCDFs), polychlorinated biphenyls (PCBs), and organochlorine (OC) pesticides were measured in unsuccessfully hatched eggs of three different kinds of predatory birds: 3 eggs of sparrowhawks, 7 eggs of hobbies, and 16 eggs of goshawks collected in the German region of Berlin-Brandenburg.Using toxic equivalency factors for birds, eggs of hobbies contained mean concentrations of 478 pg TEQ/g fat and 551 pg TEQ/g fat contributed by PCDD/Fs and coplanar PCBs, respectively. For sparrowhawks the respective TCDD equivalents were 424 and 1278 pg/g fat; those for goshawks were 211 and 935 pg/g fat. The mean value of the summed concentrations of the PCB congeners 28, 52, 101, 138, 153, and 180 amounted to 11 μg/g fat in eggs of hobbies, 9.5 μg/g fat for sparrowhawks, and 16.1 μg/g fat for goshawks.Of the analyzed organochlorine pesticides the concentration of p,p′-DDE was highest (up to 273 μg/g); the concentration of the other OCs, with the exception of methoxychlor in eggs of goshawks (highest level of 10.6 μg/g fat), were negligible. In all cases the calculated toxicity of the coplanar PCBs surpassed the toxicity of the PCDD/Fs, at least by a factor of two. Due to the higher concentration of the coplanar PCB 77 compared to PCB 126 in eggs of hobbies, it is concluded that its metabolic excretion in this species is much lower than in sparrowhawks and goshawks. Received: 25 May 2001/Accepted: 10 December 2001  相似文献   

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