Recommendations for Monitoring of Polybrominated Diphenyl Ethers in the Canadian Environment

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.     

焦化、染料废水和洹河水体的有机污染研究

采用GC/MS联用仪对焦化、染料废水和地表水中有机物进行定性、定量分析,探讨了污染源与受纳区的地表水中有机物种类和含量间的关系。     

城市污水处理厂水样中菊酯类农药残留分析

建立了基于C18固相萃取柱和气相色谱/电子捕获(GC/ECD)分析水体中环境激素类物质——菊酯类农药的分析方法,并对方法的回收率、灵敏度进行了评价,同时分析了北京市高碑店、北小河两个城市污水处理厂进水与出水中菊酯类农药的浓度,研究发现在其废水中存在联苯菊酯、氯氰菊酯、氰戊菊酯和溴氰菊酯,浓度在0.013~0.920μg/L之间。结果表明,曝气活性污泥法对菊酯类农药的去除效果较好。方法对菊酯类农药的回收率达到67.7%~96.2%,方法检测限为0.010~0.015μg/L。     

污水中新精神活性物质的分析方法优化及验证

随着对传统毒品打击力度的增大,各种为规避现行法律管制而合成的新精神活性物质(new psychoactive substances,NPS)层出不穷.NPS被滥用后,经人体新陈代谢所生成的代谢产物和未被代谢的原药随尿液进入生活污水,从而汇入污水处理厂,经处理后被排入自然水体.因此在国内外以往相关研究的基础上,应用固相萃取和UPLC-MS/MS技术,建立并优化了污水中11种常见NPS的前处理及检测方法.比较了污水前处理条件(如SPE柱、样品p H值、淋洗和复溶等)对目标物回收率的影响.结果表明最优前处理条件为:选用Oasis MCX柱,在p H=2的条件下加载样品,用2 m L p H=2的超纯水和2m L甲醇淋洗SPE柱,400μL 20%的甲醇水溶液复溶.通过对目标物的保留时间、回收率、基质效应、检出限和定量限、精密度等指标的评价,说明优化后的前处理方法和C18-UPLC-MS/MS检测方法高效可靠.应用优化后的方法对北京市11家污水处理厂的进、出水样进行了分析,验证了方法的可靠性,为进一步开展NPS的污水流行病学研究及健康风险评价提供了参考依据.     

超高效液相色谱-串联四级杆质谱法快速测定阿特拉津、甲萘威、微囊藻毒素LR、丙烯酰胺和联苯胺

以地表水环境质量标准为依据,建立了直接进样-超高效液相色谱-串联四级杆质谱法快速同时测定地表水中阿特拉津、甲萘威、微囊藻毒素LR、联苯胺和丙烯酰胺的方法。水样采集后经0．22μm滤膜过滤后直接进样,使用C18反相柱为分离柱,柱温40℃,流速0．2 ml/min,乙腈和甲酸水(0．1%)作为流动相,采用梯度洗脱,串联质谱采用MRM模式,使用ESI(+)源电离水样,每个样品分析时间仅需2．5 min。五种物质检出限为0．0001~0．0003 mg/L,加标回收率为80．0%~118．9%,满足国家标准要求。针对地表水所需检测项目进行优化,提高了实验室水质检测效率,同时测定多组分且分析时间短,适用于地表水中相关项目的监测。     

吹扫捕集-GC/MS法检测饮用水中十三种常见挥发性有机物

建立了吹扫捕集-GC/MS法检测饮用水中十三种常见挥发性有机物的方法。最低检出限在0.041~1.08μg/L之间,加标回收率在80%~120%,具有较高的灵敏度和较广的分析范围。该分析方法准确、快速,能实现一针进样同时检测13种物质,缩短了分析周期,并应用该方法对城市水样进行了实测分析。     

超快速液相色谱-串联质谱法测定制药废水中阿维菌素的研究

建立了采用固相萃取-超快速液相色谱-串联质谱（SPE-RRLC-MS/MS）测定制药废水中阿维菌素残留的方法.水样经离心、沉淀蛋白质后,上清液采用HLB固相萃取柱富集和净化;以0.1%甲酸水溶液和50%～90%甲醇为流动相,采用AgilentPlusC18柱进行RRLC分离,在串联质谱ESI（＋）模式下采用多反应监测模...     

气质联用法测定空气中挥发性有机物的方法研究

通过美国Entech公司Summa罐采集大气样品,7100型大气预浓缩系统提取和富集样品中的挥发性有机物,省去了繁琐的有机物提取和净化工序,避免和有机溶剂接触,将样品直接输入气质联机进行分析。利用这种方法定性分析了某油罐区的大气成分,结果表明该地区大气中含有成分复杂的环己烷、苯和萘的衍生物,这些化合物的浓度远远大于居民区同类化合物的含量。     

噬菌体MS2生物学特性研究

本文分析了噬菌体MS2在水质监测中作为水中肠道病毒指示生物的可行性与优势,并通过试验测定了噬菌体MS2的热稳定性、pH值稳定性、最佳感染复数和一步生长曲线等生物学参数,结果表明:噬菌体MS2的热稳定性较弱,在70℃时5 min内即会全部失活;在pH值4～10的范围内噬菌体MS2均可稳定存在;噬菌体MS2感染其宿主大肠杆...     

HCH residues in point-source contaminated samples of the Teltow Canal in Berlin,Germany

Contaminated groundwater and a riverine sediment core heavily affected by the same industrial point source were analysed for hexachlorocyclohexanes (HCH) and its degradation products. A detailed quantification by GC/MS revealed contamination levels up to 730 μg/L and 396 ng/g in sum for the water and sediment samples, respectively. The isomer pattern differed significantly in both compartments. The ground water samples were depleted in γ-HCH, whereas a significant loss of α-HCH was evident in the sediments as compared to the technical composition. The data obtained revealed interesting insights into the transformation behaviour and fate of HCH mixtures in anaerobic environmental compartments. In the affected groundwater system an ongoing microbial degradation was pointed out by the identification of indicative anaerobic metabolites. On the contrary in the sedimentary system a high environmental stability or rather a hindered degradation was observed as indicated by unaltered concentration levels as compared to production rates as well as by the absence of metabolites. Interestingly, the environmental fate of HCH in subaquatic sediments as well as in anaerobic ground water differs highly in contrast to the behaviour in anaerobic soil or surface water systems. Further on, it has to be stated, that the knowledge about the long-term behaviour of HCH residues in sedimentary material under anaerobic conditions is rather limited so far.