HPLC-MS/MS法测定三角帆蚌中多种N-亚硝胺类化合物

采用基质分散固相萃取-同位素稀释-HPLC-MS/MS法同时测定三角帆蚌肉中9种N-亚硝胺类化合物(NAs),通过优化前处理和仪器条件,使方法在5.00μg/L～200μg/L范围内线性良好,方法检出限为2.58μg/kg～8.86μg/kg。对样品做2个质量比水平的加标回收试验,各组分的平均回收率为78.1%～90.3%,RSD值≤6.8%。将该方法用于测定20个河蚌样品,9种NAs均为未检出。     

N—亚硝胺的确证技术

N—亚硝胺是一种强致癌物。在空气、水、土壤及食品等环境样品中含有痕量的这种化合物。因此,对这种化合物的检测关系到人体健康的一件技术工作。对N—亚硝胺的分析方法还存在着不易确证等技术难题。当前多采用GC—MS法(气相色谱—质谱法)和HPLC—MS法(液相色谱—质谱法)。MS法是确证N-亚硝胺的唯一较可靠的分析方法。但是,由于该法操作复杂,仪器设备昂贵,使得很多实验室无能为力。可是,近十年来,N—亚硝胺的确证技术已发展为验证N—亚硝胺的表观存在了。下面介绍的几种在大多数情况下是可靠的方法:     

质谱及其联用技术在水中消毒副产物识别和分析中的应用

水中消毒副产物(DBPs)是在水消毒过程中消毒剂与水中溶解性有机物以及无机离子发生反应而产生,其对水环境生态安全和人体健康有不利影响。简述了DBPs的生成、种类、毒性和分析方法等,重点综述了气相色谱-质谱联用(GC-MS)、液相色谱-质谱联用(LC-MS)、离子色谱-质谱联用(IC-MS)以及超高分辨率质谱(UPMS)等质谱(MS)及其联用技术在水中DBPs识别和分析中的应用,分析了不同MS技术的特点和应用实例,提出了MS技术在DBPs研究领域的发展方向与挑战。     

水中粪大肠菌群快速检测方法-固定底物酶底物法与多管发酵法的比较

目的在于比较固定底物酶底物法与多管发酵法用于水中粪大肠菌群(耐热大肠菌群)的检测,使用科立得TM(Colilert(R))试刺和传统方法检测地表水、水源水及污水水样,比较固定底物酶底物法与多管发酵法用于水中粪大肠菌群(耐热大肠菌群)检测结果的一致性.结果表明,固定底物酶底物法与多管发酵法用于水中粪大肠菌群(耐热大肠菌群)检测结果具有一致性,固定底物酶底物法可以用作评价水质微生物污染的标准方法.     

高效液相色谱串联质谱法测定某市污水处理厂进出水中的全氟化合物

通过建立直接进样-高效液相色谱串联质谱（HPLC-MS/MS）测定污水处理厂进出水中的10种全氟化合物的方法，了解污水厂进出水中全氟化合物污染情况。10种目标分析物在10~500 ng/L范围内具有良好的线性关系，方法检出限为2.3~8.3 ng/L，精密度为2.1%~7.1%，加标回收率为60.6%~91.7%。应用该方法测定某市典型污水厂进出水中的全氟化合物，进水中全氟化合物质量浓度为90.9~206 ng/L，主要污染物是PFOA、PFHxS和PFBS；出水中全氟化合物的质量浓度为67.4~158 ng/L，环境排放量为6.7~22.9 g/d，主要污染物是PFOA和PFHxS。结果表明，该方法能很好地适用于复杂基质中10种全氟化合物的检测。     

陕西省城镇污水处理厂进出水中主要离子与重点元素分布特征

污水处理厂出水中主要离子和重点元素的浓度特征及去除效果会影响受纳水体的盐度、碱度等指标,从而影响河湖的生态服务功能,但是这方面的研究长期以来未得到充分关注。在陕西省全境选择51家城镇污水处理厂,测定进水和出水中的钾、钙、钠、镁、氟、氯和硫酸根离子,以及铁、锰、硼、钼、锶等重点元素的浓度。测定结果显示:陕西省城镇污水处理厂进水和出水中的阳离子以钠离子为主,其次是钙、镁离子,钾离子浓度最低;阴离子中,氯离子浓度最大,其次为硫酸根离子。就总离子浓度而言,陕北和关中地区污水处理厂进水的离子浓度普遍高于陕南地区。相关性分析结果显示:在污水处理厂进水中,钠、氟、氯、镁及硫酸根离子相互之间均呈现显著正相关关系;铁、锰在进水中没有表现出明显的相关关系,而在出水中呈现显著的正相关关系。污水处理厂仅能够处理污水中少量的氟、钾和镁离子。铁元素和锰元素在经过污水处理厂的处理后,浓度有所升高。此研究的研究结果可为河湖水化学组成管理决策提供参考。     

两种酶底物法监测水中(粪)大肠菌群商品化制品的比较

比较了进口colilert试剂和国产colitech试剂及其各自配套制品对水中(粪)大肠菌群的检测,包括总大肠菌群和粪大肠菌群。分别使用同为酶底物法的两种制品检测地表水、地下水、水源水、生活饮用水及污水水样,比较了两种制品用于水中(粪)大肠菌群检测结果的一致性,同时验证了两种制品的无菌性和培养基的选择性。试验结果表明,进口colilert试剂和国产colitech试剂及其各自配套制品于水中(粪)大肠菌群检测结果具有一致性,培养基具有很好的选择性。     

饮用水消毒副产物检测技术应用进展

饮用水消毒副产物是水体进行消毒过程中天然有机物与消毒剂反应生成的副产物。毒理学和流行病学相关研究表明,饮用水消毒副产物会对人体健康产生不利影响。笔者综述了传统与新兴消毒副产物检测过程中的前处理技术与分析技术,总结了不同前处理技术和分析技术的原理、优缺点及应用情况,并预测和展望了消毒副产物检测技术的发展前景。     

典型化工污水处理厂废水及受纳水体的生物急性毒性监测方法应用研究

为了研究生物急性监测方法对监测典型化工污水处理厂废水的适用性,选择2家常州市典型的化工园区污水处理厂("常A"和"常B"),进行了发光细菌、藻类、大型溞和斑马鱼卵4种不同层次受试生物的急性毒性检测。研究表明,发光细菌急性毒性、藻类叶绿素荧光毒性在2个污水处理厂中均被检测到,发光细菌急性毒性通常进水大于出水,但在投放大量氧化消毒剂时,出水表现出剧毒。藻类叶绿素荧光毒性最高值出现在常B进水中。大型溞和斑马鱼卵急性毒性仅在常B进出水样中有检出,受纳河道下游水样虽未表现出急性毒性,但可观察到斑马鱼卵各类发育畸形。4种生物急性毒性检测方法中,发光细菌适用范围最广,藻类、大型溞和斑马鱼卵急性毒性方法可根据监测目的和工业园区特点相应选择。实验结论可为化工污水处理厂尾水排放过程中生物毒性监测的常态化提供方法选择,为管理部门制定排放标准提供依据。     

在线液液萃取-气相色谱-质谱法测定生活饮用水中卤代乙腈

优化建立了在线液液萃取-气相色谱-质谱法测定饮用水中7种卤代乙腈的方法。通过多功能在线进样装置,研究设计了在线液液萃取的技术流程,优化了液液萃取关键参数,并建立了气相色谱-质谱检测方法。该方法对氯乙腈、二氯乙腈、三氯乙腈、溴乙腈、二溴乙腈、溴氯乙腈和碘乙腈等7种卤代乙腈都有较好的检测灵敏度,方法检测限为0.1~0.8 μg/L,纯水中高浓度加标回收率为72.0%~91.4%,精密度为1.8%~3.9%。经技术对比和应用验证,该方法具有高效灵敏、简便快速等特点,样品检测无干扰,自动化程度高,适用于饮用水中卤代乙腈类消毒副产物的检测。     

饮用水消毒副产物--卤乙酸的检测

卤乙酸是饮用水氯化消毒中一类主要的消毒副产物,由于存在的广泛性和潜在的健康危害,许多国家和卫生组织相继将其列为饮用水常规监测项目,而我国至今还没有相关规定;为了更好地控制饮用水中卤乙酸的形成,世界各国科研人员先后研究和开发出了性能逐趋完善的多种分析检测方法;本文在国内外文献调研的基础上,对卤乙酸的各种分析检测方法进行了简要的介绍,并指明了今后的发展方向.     

Ascorbic acid reduction of residual active chlorine in potable water prior to halocarboxylate determination

In studies on the formation of disinfection byproducts (DBPs), it is necessary to scavenge residual active (oxidizing) chlorine in order to fix the chlorination byproducts (such as haloethanoates) at a point in time. Such research projects often have distinct needs from requirements for regulatory compliance monitoring. Thus, methods designed for compliance monitoring are not always directly applicable, but must be adapted. This research describes an adaptation of EPA Method 552 in which ascorbic acid treatment is shown to be a satisfactory means for reducing residual oxidizing chlorine, i.e., HOCl, ClO-, and Cl2, prior to determining concentrations of halocarboxylates. Ascorbic acid rapidly reduces oxidizing chlorine compounds, and it has the advantage of producing inorganic halides and dehydroascorbic acid as opposed to halogenated organic molecules as byproducts. In deionized water and a sample of chlorinated tap water, systematic biases relative to strict adherence to Method 552 were precise and could be corrected for using similarly treated standards and analyte-fortified (spiked) samples. This was demonstrated for the quantitation of chloroethanoate, bromoethanoate, 2,2-dichloropropanoate (dalapon), trichloroethanoate, bromochloroethanoate, and bromodichlorocthanoate when extracted, as the acids, into tert-butyl methyl ether (MTBE) and esterified with diazomethane prior to gas chromatography with electron capture detection (GC-ECD). Recoveries for chloroethanoate, bromoethanoate, dalapon, dichloroethanoate, trichloroethanoate, bromochloroethanoate, bromodichloroethanoate, dibromoethanoate, and 2-bromopropanoate at concentrations near the lower limit of detection were acceptable. Ascorbic acid reduction appears to be the best option presently available when there is a need to quench residual oxidants fast in a DBP formation study without generating other halospecies but must be implemented cautiously to ensure no untoward interactions in the matrix.     

饮水中挥发性卤代烃成因研究

对影响饮水生成挥发性卤代烃的各种因素进行了研究.发现源水腐殖质等有机物的存在和加氯消毒处理是产生挥发性卤代烃的主要原因,而氯化消毒的温度、时间、源水pH值对其生成有重要影响.     

Urban stormwater harvesting and reuse: a probe into the chemical, toxicology and microbiological contaminants in water quality

Stormwater is one of the last major untapped urban water resources that can be exploited as an alternative water source in Australia. The information in the current Australian Guidelines for Water Recycling relating to stormwater harvesting and reuse only emphasises on a limited number of stormwater quality parameters. In order to supply stormwater as a source for higher value end-uses, a more comprehensive assessment on the potential public health risks has to be undertaken. Owing to the stochastic variations in rainfall, catchment hydrology and also the types of non-point pollution sources that can provide contaminants relating to different anthropogenic activities and catchment land uses, the characterisation of public health risks in stormwater is complex, tedious and not always possible through the conventional detection and analytical methods. In this study, a holistic approach was undertaken to assess the potential public health risks in urban stormwater samples from a medium-density residential catchment. A combined chemical–toxicological assessment was used to characterise the potential health risks arising from chemical contaminants, while a combination of standard culture methods and quantitative polymerase chain reaction (qPCR) methods was used for detection and quantification of faecal indicator bacteria (FIB) and pathogens in urban stormwater. Results showed that the concentration of chemical contaminants and associated toxicity were relatively low when benchmarked against other alternative water sources such as recycled wastewater. However, the concentrations of heavy metals particularly cadmium and lead have exceeded the Australian guideline values, indicating potential public health risks. Also, high numbers of FIB were detected in urban stormwater samples obtained from wet weather events. In addition, qPCR detection of human-related pathogens suggested there are frequent sewage ingressions into the urban stormwater runoff during wet weather events. Further water quality monitoring study will be conducted at different contrasting urban catchments in order to undertake a more comprehensive public health risk assessment for urban stormwater.     

地下水采样方法比对研究

选取3种地下水采样方法开展方法比对研究。通过系统分析监测数据,指出了3种方法所采水样在基本水质参数、无机离子、金属、挥发性有机物以及感官类指标等项目监测上的显著差异,指出了各种方法的适用性并分析原因。结果表明:与贝勒管法、潜水泵法相比,低流速法有效地解决了采样操作过程中易产生的曝气问题;对井内水体扰动较小,降低了水样浊度;减小了井内水位的大幅度泄降,避免了不同层位间污染物的迁移及周边水和井内滞水的交叉污染;节约了场地操作时间和后期污水处理所需花费。因此,低流速法在采取代表性水质样品方面更具方法优势。     

Formation and modeling of disinfection by-products in drinking water of six cities in China

Water quality parameters including TOC, UV(254), pH, chlorine dosage, bromide concentration and disinfection by-products were measured in water samples from 41 water treatment plants of six selected cities in China. Chloroform, bromodichloromethane, dibromochloromethane, dichloroacetic acid and trichloroacetic acid were the major disinfection by-products in the drinking water of China. Bromoform and dibromoacetic acid were also detected in many water samples. Higher concentrations of trihalomethanes and haloacetic acids were measured in summer compared to winter. The geographical variations in DBPs showed that TTHM levels were higher in Zhengzhou and Tianjin than other selected cities. And the HAA5 levels were highest in Changsha and Tianjin. The modeling procedure that predicts disinfection by-products formation was studied and developed using artificial neural networks. The performance of the artificial neural networks model was excellent (r > 0.84).     

Bromate analysis in groundwater and wastewater samples

Bromate (BrO(3)(-)) is a disinfection by-product formed during ozonation of potable water supplies containing bromide (Br(-)). Bromate has been classed by the World Health Organisation as a 'possible human carcinogen', leading to implementation of 10-25 microg L(-1)(as BrO(3)(-)) drinking water limits in legislative areas including the United States and European Union. Techniques have been developed for bromate analysis at and below regulatory limits, with Ion Chromatography (IC) coupled with conductivity detection (IC-CD), post-column reaction and ultra-violet (UV) detection (IC-PCR), or inductively coupled plasma-mass spectrometry detection (IC-ICPMS) in widespread use. The recent discovery of bromate groundwater contamination in a UK aquifer has led to a requirement for analysis of bromate in a groundwater matrix, for environmental monitoring and development of remediation strategies. The possibility of bromate-contaminated water discharge into sewage treatment processes, whether accidental or as a pump-and-treat strategy, also required bromate analysis of wastewater sources. This paper summarises techniques currently available for trace bromate analysis in potable water systems and details studies to identify a methodology for routine analysis of groundwater and wastewater samples. Strategies compared were high performance liquid chromatography (HPLC) with direct UV or PCR/UV detection, IC-CD, IC-PCR, and a simple spectrophotometric technique. IC-CD was the most cost-effective solution for simultaneous analysis of bromate and bromide within groundwater samples, having a 5 microg L(-1) detection limit of both anions with limited interference from closely-eluting species. Wastewater samples were successfully analysed for bromate only using HPLC with PCR/UV detection, with detection limits below 20 microg L(-1)(as BrO(3)(-)) and low interference. HPLC with direct UV detection was unsuitable for bromate analysis within the concentration range 50-5000 microg L(-1) which was required for this project, but column choice was shown to be a major factor in determining limits of detection. Spectrophotometry could not reproducibly determine bromate concentration, although the technique showed promise as a quick field method for high-level groundwater bromate analysis.     

Modeling the Formation of Chlorination By-Products During Enhanced Coagulation

Because of increasing need to balance health risks for pathogen control and disinfection by-products (DBP) formation in drinking water supplies, water utilities are forced to closely examine and optimize their disinfection practices. This research was designed to investigate the effects of independent variables of dissolved organic carbon (DOC), ferric chloride dosage, chlorine dose, and reaction time on trihalomethanes (THMs) formation in Terkos Lake Water (TLW) of Istanbul City. A statistically-based empirical model was developed for predicting THM formation during enhanced coagulation. The R ² and F value of model were 0.762 and 460, respectively. The model was found to be statistically significant for all four variables, and model predictions appear to be most accurate for this study. A multiple linear model exhibited the best fit of data. It was observed that THM formation depended primarily on DOC removal. Model calibration, testing and validation were accomplished by using independent data set.