多类持久性有机污染物同时分析方法及应用

发布时间：2018-04-20 14:11

本文选题：持久性有机污染物 + HRGC-HRMS　；参考：《河北师范大学》2017年硕士论文

【摘要】：持久性有机污染物(Persistent Organic Pollutants,POPs)是一类在环境中难降解、在生物体内难代谢,具有很强的亲脂性,可以在食物链中富集,能够通过蒸发-冷凝等过程远距离传输的污染物,该类污染物毒性高,即使在微量水平也能对生态环境和人体健康产生显著不良影响。针对环境样品中痕量有机物分析的样品前处理的繁琐费时以及痕量污染物之间的测定干扰,建立了沉积物和生物样品中多氯联苯(PCBs),二VA英(PCDD/Fs,多溴联苯醚(PBDEs),溴代二VA英(PBDD/Fs),多氯萘(PCNs),有机氯(OCPs),短链氯化石蜡(SCCPs),德克隆(DP)八类持久性有机物同时分析的方法。样品采用加速溶剂萃取,多层复合硅胶柱、碱性氧化铝柱和弗罗里硅土柱净化分离,根据各类物质的性质,选择色谱柱和检测器进行定性定量分析。方法检出限范围为0.1-30pg/g(鱼组织),0.133pg/g(沉积物),SCCPs除外。回收率范围为:43%-120%(鱼组织),45%-115%。精密度小于33%。方法准确可靠,用于标准参考物质1941b,WMF-01中的PCBs、PCDD/Fs、PBDEs和OCPs的测定,测定结果均在参考值范围内。对白洋淀水和沉积物中的持久性有机污染物的污染水平、指纹分布进行了分析研究。结果表明:白洋淀沉积物和水中的PCBs的浓度分别为0.55-241.3ng/g和ND-27.4ng/L,中值浓度分别为27.6ng/g和1.44 ng/L。PCDD/Fs的浓度分别为3.6-4093.7pg/g,中值浓度为0.63ng/g。PCNs的浓度分别为0.030-1.56ng/g,0-650.3ng/L,中值浓度分别为0.37ng/g和7.84ng/L。PBDEs的范围为0.080-8599.9ng/g和0.39-6.07ng/L,中值浓度分别为3.26ng/g和1.11ng/L。水中和沉积物中以四氯代、五氯代、六氯代的PCBs为主,占PCBs总量的90%。水中检测出PCB138、38、151、132、160、179、187、174、180、209,总浓度为0.09ng/L,占PCBs总量的6.52%。与国内外湖泊相比,污染水平较低。沉积物中主要以PCB101、118、153、138、180、52为主要同类物,百分比为90%,浓度为8.67ng/g干重,与国内外湖泊相比,污染水平较低。沉积物中PCDD/Fs的浓度范围为3.6pg/g-4093.7pg/g,与国内外湖泊相比,PCDD/Fs污染处于中等水平。水中PCNs主要以一氯代和四氯代污染为主,沉积物中以三氯代至八氯代为主;与国内外各湖泊PCNs的污染水平相比,污染水平较低。水中主要检测出10种PBDEs同类物,BDE-28、37、75、49、47、66、116、153、166、138。韩国Shihwa湖、巢湖、太湖中PBDEs含量范围为1.3ng/g-18700ng/g、236.7ng/g-1373.4ng/g、0.39ng/g-34.44ng/g;沉积物中的PBDEs以BDE-30、47、49和209为主。厦门沿岸和{|{\湖、红枫湖、Hadley湖(美国)、百花湖沉积物中PBDEs的含量范围为0.42ng/g-10.57ng/g、ND-9.04ng/g、5.20ng/g-37.6ng/g、0.42ng/g-3.14ng/g,水中PBDEs的污染较轻,沉积物中污染严重。
[Abstract]:Persistent Organic Pollutants (pops) is a class of pollutants that are difficult to degrade in the environment, difficult to metabolize in organisms, highly lipophilic, can be enriched in the food chain and can be transported remotely through processes such as evaporation-condensation, etc. This kind of pollutant is highly toxic and can have significant adverse effects on the ecological environment and human health even at the micro level. In view of the tedious and time-consuming pretreatment of samples for the analysis of trace organic matter in environmental samples and the interference in the determination of trace pollutants, A method was established for simultaneous analysis of eight persistent organic compounds in sediments and biological samples: PCBsO, DVA, PCDDR / Fs, PBDEsN, PBDDD / FsN, PCNsN, OCPsN, SCCPsS, DPX). The samples were purified and separated by accelerated solvent extraction, multilayer composite silica gel column, alkaline alumina column and Flory silica column. The chromatographic column and detector were selected for qualitative and quantitative analysis according to the properties of various substances. The detection limit was 0.1-30pg / g (fish tissue 0.133pg / g) (with the exception of sediment SCCPs). The recoveries range from: 43 to 120. The precision is less than 33. The method is accurate and reliable, and has been applied to the determination of PCBsN PCDDR / FsN PBDEs and OCPs in the standard reference substance 1941 BX WMF-01. The results are within the range of reference values. The pollution level and fingerprint distribution of persistent organic pollutants in Baiyangdian water and sediment were studied. The results show that the concentration of PCBs in sediment and water of Baiyangdian is 0.55-241.3ng/g and ND-27.4ng / L, the median concentration of 27.6ng/g and 1.44 ng/L.PCDD/Fs is 3.6-4093.7pg / g, the median concentration of 0.63ng/g.PCNs is 0.030-1.56ng / g / g 0-650.3ng / L, the range of median concentration is 0.37ng/g and 7.84ng/L.PBDEs, respectively. The median concentrations of 0.080-8599.9ng/g and 0.39-6.07ng / L were 3.26ng/g and 1.11ng / L, respectively. In water and sediment, tetrachloro, pentachlorinated, hexachlorinated PCBs is the dominant, accounting for 90% of the total PCBs. PCB 138C 381532160179187174180209 was detected in water with a total concentration of 0.09ng / L, which accounted for 6.52% of the total PCBs. Compared with domestic and foreign lakes, the pollution level is lower. In sediments, PCB 101118153138180% was the main congener, the percentage was 90 and the concentration was 8.67ng/g dry weight. The pollution level was lower than that in domestic and foreign lakes. The concentration of PCDD/Fs in sediments ranged from 3.6 PG / g to 4093.7 PG / g, and the pollution of PCDDFs was at a medium level compared with that of lakes at home and abroad. PCNs in water is mainly polluted by monochlorination and tetrachlorohydrin, and in sediment by trichlorooctachlorination, and the pollution level is lower than that of PCNs in lakes at home and abroad. Ten species of PBDEs congeners were mainly detected in water. The range of PBDEs content in Shihwa Lake, Chaohu Lake and Taihu Lake in South Korea is 1.3ng / g-18700ng / g, 236.7ng / g-1373.4ng / g / g, 0.39ng / g-34.44ng / g respectively, and the PBDEs in sediment is mainly BDE-30 / 47ng / g ~ (49) and 209ng / g. Along the coast of Xiamen and {{{\ Lake, Hongfeng Lake] Hadley Lake (USA, Baihua Lake) contains PBDEs in the range of 0.42ng / g-10.57ng / r / g ND-9.04ng / g / g = 5.20ng / g-37.6ng / g / g 0.42 ng / g / g / g respectively. The pollution of PBDEs in water is light, and the pollution in sediment is serious.
【学位授予单位】：河北师范大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：X132;O652

【相似文献】