高效液相色谱-串联质谱法分析水体中六溴环十二烷异构体

建立了高效液相色谱-串联质谱(HPLC-MS-MS)准确测定水体中六溴环十二烷(HBCD)3种异构体(α-HBCD、β-HBCD、y-HBCD)残留量的方法.样品添加13C-HBCD后,以二氯甲烷液液萃取,萃取液经硅胶柱净化后,以甲醇-0.2％氨水溶液为流动相通过BDS-C18色谱柱进行分离,采用电喷雾电离(ESI)、负离子模式对HBCD异构体进行分析.该方法线性范围为0.5 ～ 100 μg/L,α-HBCD、β-HBCD、γ-HBCD 3种异构体检出限分别为0.42、0.52、0.48 ng/L,平均回收率分别为88％、84％、86％,相对标准偏差均小于6.5％.应用该法对黄海沿岸21个采样站位水样进行分析,其中13个采样站位有HBCD 3种异构体的检出,表明该法适用于水体中HBCD的检测.     

液相色谱-质谱法测定土壤中四溴双酚A和六溴环十二烷

文章建立了液相色谱-串联四级杆质谱仪同时测定土壤中四溴双酚A及3种六溴环十二烷同分异构体的分析方法。土壤样品经快速溶剂仪萃取,全自动凝胶净化系统净化后,使用液相色谱-串联四级杆质谱仪,负离子电喷雾多反应监测模式监测,内标法定量分析。结果表明,土壤中四溴双酚A、α-六溴环十二烷、β-六溴环十二烷和γ-六溴环十二烷的检出限为0.1~1.2 pg/g,加标回收率为81.8%~113%,相对标准偏差小于10%。该方法分析时间短,灵敏度高,操作简单,对电子固废拆解场地中的179个土壤样品进行分析,取得满意结果。     

QuEChERS-超高效液相色谱-串联质谱法测定鱼肉中六溴环十二烷

建立了一种测定鱼肉中六溴环十二烷（HBCD）的QuEChERS-超高效液相色谱-串联质谱方法。方法采用QuEChERS法进行样品前处理,采用C18色谱柱分离,以水为流动相A,以甲醇-乙腈（V∶V=50∶50）为流动相B进行梯度洗脱;采用超高效液相色谱-串联质谱法在负离子模式下以多反应监测方式检测,用同位素稀释法定量。该方法在 0.5~50μg/L范围内具有良好的线性关系（相关系数≥0.999）,检出限为0.05~0.27 μg/kg,3个加标质量分数（2.5,125,25 μg/kg）的回收率范围为99.3%~107%,相对标准偏差为0.4%~8.4%。该方法简便准确、灵敏度高,可满足鱼肉中HBCD的检测要求。     

高效液相色谱串联三重四极杆质谱测定地表水中六溴环十二烷和四溴双酚A

通过考察固相萃取条件,优化色谱质谱参数,建立了一种可靠、灵敏的新方法测定地表水中六溴环十二烷(HBCD)和四溴双酚A(TBBPA)。方法采用固相萃取小柱(HLB)萃取,10 mL正己烷/二氯甲烷(体积比1∶9)、甲醇(5mL)依次洗脱,以ACQUITY UPLC BEH C₈为色谱柱,甲醇/水溶液为流动相,流速0.3 mL/min进行梯度洗脱,采用大气压化学电离(APCI)源离子化、多反应监测模式(MRM)测定,同位素稀释内标法定量。四溴双酚A和六溴环十二烷的方法检出限为4~13 pg/L,测定下限为16~52 pg/L,地表水加3个浓度水平标准物质回收率为53.0%~104%,相对标准偏差为3.2%~18%(n=5)。将该法应用于沱江流域17个地表水样分析,TBBPA和HBCD部分样品有检出,检出质量浓度为未检出~1 087 pg/L。     

超高效液相色谱-串联质谱法同时检测溴代阻燃剂

采用Acquity BEH C18色谱柱,以甲醇-乙腈混合液和水为流动相,辅以电喷雾正离子模式多反应监测(MRM)进行定性定量分析,建立了一种同位素稀释超高效液相色谱-串联质谱(UPLC-MS/MS)同时检测四溴双酚A(TBBPA)、三-(2,3-二溴丙基)异氰脲酸酯(TBC)和3种六溴环十二烷(HBCD)异构体的方法。水样通过固相萃取进行净化,回收率达到85.3%~96.1%。土壤和底泥样品经加速溶剂萃取后,采用酸性硅胶和中性硅胶柱进行净化,回收率达到81.5%~102.7%。该方法对TBBPA、TBC、α-HBCD、β-HBCD、γ-HBCD在水和土壤中的检测限分别为1.0、1.2、2.0、0.8、1.2 ng/L和0.10、0.12、0.20、0.08、0.12 ng/g。     

固相萃取-超高效液相色谱-串联质谱法测定水中6种雌激素

建立了固相萃取-超高效液相色谱-串联质谱(SPE-UPLC-MS-MS)同时检测水样中6种雌激素(壬基酚、双酚A、雌酮、17α-雌二醇、17α-乙炔雌二醇、雌三醇)的方法.样品采用SPE小柱富集后,用90％乙腈-0.1％氨水混合溶液洗脱浓缩定容.在梯度洗脱条件下,6种雌激素用三重四极杆串联质谱检测.该方法显示出良好的线性关系(r ＞0.999)和精密度(RSD＜ 10％),方法检出限为1.3 ～5.2 ng/L.该方法成功应用于地表水、地下水和废水样品中6种雌激素分析,样品加标回收率为76.8％～117％.该方法准确、灵敏、无需衍生,可用于同时测定水样中的6种雌激素.     

在线固相萃取-高效液相色谱-串联质谱法测定饮用水中4种兴奋剂

可替宁、可待因、1,7-二甲基黄嘌呤和咖啡因作为药物及其代谢产物广泛应用于日常生活中,其在环境中的残留物可能对人类健康和生态环境安全造成威胁。采用在线固相萃取法进行前处理,酸性条件(0.1%甲酸水溶液)上样,水样加硫代硫酸钠(1L水样加0.1g硫代硫酸钠)除去余氯后用高效液相色谱-串联质谱法测定饮用水中可替宁、可待因、1,7-二甲基黄嘌呤和咖啡因这4种兴奋剂。当进样体积为1.0mL时,方法检出限为0.633~1.75ng/L,测定下限为2.53~6.98ng/L,饮用水样品加标回收率为80.0%~129%,多次测定均值的相对标准偏差(RSD)<5%。方法检出限低,精密度和准确度好,能满足饮用水样品中4种兴奋剂的日常检测。     

固相萃取-液相色谱-串联质谱法测定水中5种雌激素

建立了固相萃取-液相色谱-串联质谱组合联用技术同时测定地表水、饮用水和污水处理厂出厂水中的5种雌激素(17β-雌二醇、雌三醇、雌酮、17α-炔雌醇、己烯雌酚)的方法。水样经过全自动固相萃取仪富集,以OASIS HLB柱为萃取柱,甲醇为洗脱剂,用液相色谱-串联四极杆质谱联用仪分析定量。分别在0.5~8、5~80μg/L范围内线性良好,相关系数为0.995~0.998。17β-雌二醇、雌三醇、17α-炔雌醇的检出限均为5μg/L,雌酮与己烯雌酚的检出限为0.5μg/L。5种雌激素的纯水加标回收率为63.6%~120.2%,地表水加标回收率为59.8%~91.5%,自来水加标回收率为55.3%~92.1%,精密度为3.7%~10.7%,该方法简单、可靠,可用于水中雌激素类污染物的同时测定。     

超高效液相色谱-串联质谱法测定饮用水源水中磺胺类抗生素

建立了饮用水源水中6种磺胺类抗生素的固相萃取超高效液相色谱-串联质谱分析方法.优化了固相萃取、液相色谱、串联质谱多反应监测模式检测的相关参数;采用外标法定量,并对实际饮用水源水样品的基体效应进行评价.实验结果表明,目标化合物在1.0～100.0 μg/L范围内线性关系良好,仪器检出限为0.03～0.54 μg/L,实际水样的加标回收率60％ ～ 75％.该本方法灵敏度高,选择性好,外标法定量准确性较好,但实际样品存在一定的基体抑制效应.     

在线固相萃取-液相色谱-串联质谱法直接测定水中15种全氟烷基化合物

通过优化样品保存、前处理、分析条件,建立了水中15种典型全氟烷基化合物(PFASs)在线固相萃取-液相色谱-串联质谱分析方法,并对饮用水水源地和末梢水中PFASs进行定量检测。水样过膜后,准确移取700 μL水样、300 μL甲醇至1.5 mL聚丙烯进样瓶,并加入同位素内标后直接进样800 μL至在线固相萃取流路,进行萃取富集,再通过十通阀切换将洗脱的PFASs转移至分析流路进行分离,质谱检测,内标法定量。方法分析总时长22 min,15种全氟烷基化合物的方法检出限为0.31~1.20 ng/L,纯水高、中、低浓度加标样品回收率为70%~115%,相对标准偏差为0.2%~14.0%(n=6)。经实际样品验证,该方法与传统手动固相萃取方法分析结果基本一致。结果表明,该方法操作简单、自动化程度高、有机试剂用量少、灵敏度高、方法稳定,可满足地表水和末梢水中PFASs的快速测定。     

液相色谱-质谱法同时快速测定地表水中13种农药残留

通过实验建立了一种同时、快速测定地表水中13种农药残留的液相色谱-质谱分析方法。该方法采用水样直接进样,样品仅需0.5 m L,8 min完成1个样品13种农药的同时分析。方法检出限为0.1~11.5μg/L,当样品个数为7,加标量依次为10.0、40.0、100.0μg/L时,方法 RSD为2.51%~12.9%、2.09%~11.4%、1.24%~9.79%,方法准确度为82.1%~112%、92.2%~114%、93.7%~127%。对珠江三角洲地区典型的农业面源、湖泊、地表水饮用水源地等共3大类65个监测点位取样分析,以验证方法的实际可行性,监测结果符合污染物分布规律,水质整体状况良好。除甲基对硫磷外,该方法可以完全满足国家对于地表水、生活饮用水相关指标标准限值的要求,适合地表水水质农药污染状况的快速筛查监测。     

A New Mathematical Approach in Environmental and Life Sciences: Gene–Environment Networks and Their Dynamics

An important research area in life sciences is devoted to modeling, prediction, and dynamics of gene-expression patterns. As clearly understood in these days, this enterprise cannot become satisfactory without acknowledging the role of the environment. To a representation of past, present, and most likely future states, we also encounter measurement errors and uncertainties. This paper surveys and improves recent advances in understanding the foundations and interdisciplinary implications of the newly introduced gene–environment networks, and it integrates the important theme of carbon dioxide emission reduction into the networks and dynamics. We also introduce some operational and managerial issues of practical working and decision making, expressed in terms of sliding windows, quadrants (modules) of parametric effects, and navigating (controlling) between such effects and directing them. Given data from DNA microarray experiments and environmental records, we extract nonlinear ordinary differential equations that contain parameters that have to be determined. For this, we employ modern (Chebychevian) approximation and (generalized semi-infinite) optimization. After this is provided, time- discretized dynamical systems are studied. A combinatorial algorithm with polyhedra sequences allows to detect the region of parametric stability. Finally, we analyze the topological landscape of gene–environment networks with its structural (in)stability. By embedding as a module and investigating CO₂ emission control and figuring out game theoretical aspects, we conclude. This pioneering work is theoretically elaborated, practically devoted to health care, medicine, education, living conditions, and environmental protection, and it invites the readers to future research.      

微波消解-原子吸收光度法测定土壤中铜锌铅镉镍铬

用微波消解－原子吸收光度法测定土壤中铜,锌,铅,镉,镍和铬。通过硝酸－氢氟酸－过氧化氢体系消解液对土壤样品消解,选择出微波最佳消解条件。对硝酸－盐酸－过氧化氢体系消解液和硝酸－氢氟酸－过氧化氢体系消解液进行消解对比试验,发现前者不能将土壤样品完全消解,后者能将样品消解完全,但需将消解液中剩余的酸赶尽,否则测定结果将明显偏低。微波消解土壤与传统电热消解相比,操作简便快速,可提高工作效率。     

Assessing health consequences in an environmental impact assessment: The case of Amsterdam Airport Schiphol

In this article a comprehensive approach for the evaluation of possible health effects in an environmental impact assessment (EIA) is described, illustrated with the example of Amsterdam Airport Schiphol. Unlike many EIAs, we estimated quantitatively the impact of aircraft-related pollution in terms of the number of affected people for aircraft noise annoyance, odour annoyance and hypertension. In addition, an analysis of health registry data on cardiovascular and respiratory diseases and a short survey on annoyance and risk perception were carried out. The scope of a health impact assessment depends on the situation, available knowledge and data, concern in the population about the impact and the number of people concerned. It is important to pay attention to the perception of risks and concerns from all parties involved. Moreover, the results demonstrate that far more people outside the area for which standards apply were affected than inside.     

Contaminant Profiles of Two Species of Shorebirds Foraging Together at Two Neighboring Sites in South San Francisco Bay, California

The San Francisco Bay estuary isused by over one million shorebirds during springmigration and is home to several hundred thousandduring the winter. Most shorebird use occurs in thesouthern reach of the estuary (South Bay). Thereduced water circulation and discharge fromindustrial sources in the South Bay are responsiblefor the highest levels of some trace elements in theestuary. Wintering shorebirds have been found to havestrong site fidelity to areas as small as a fewkilometers in the South Bay, which may increase theirexposure to contaminants near local point sources. Inaddition, different shorebird species foraging at thesame site have been shown to have differentcontaminant burdens. Thus, our objectives were totest whether contaminant burdens differed by species,or whether contaminant burdens differed in shorebirdscollected at adjacent sites. We examined thecontaminant profiles of two species of shorebirds,long-billed dowitchers (Limnodromus scolopaceus)and western sandpipers (Calidris mauri) thatforage together at two sites, Hayward and Newark,separated by 8 km in the South Bay. We usedmultivariate analysis of variance tests to compare thecomposition of 14 elemental analytes in their livertissues and estimated their molar ratios of Hg and Se. Composite samples were used for contaminant analysesbecause of the small body size of the shorebirds. Seven elemental analytes (Ag, Ba, Be, Cr, Ni, Pb, V)were below detection limits in a majority of thesamples so statistical analyses were precluded. Inthe measurable analytes (As, Cd, Cu, Hg, Mn, Se, Zn),we found no significant intra-site differences ofcontaminant profiles for the two species. We pooledthe samples to examine inter-site differences andfound significant differences in contaminant profilesbetween shorebirds at the neighboring sites (P = 0.03). Shorebirds at Newark had higher (P < 0.05) concentrations of As, Cd, and Se than those at Hayward. Dowitchers at Newark had concentrations of Hg and Se which were highly correlated (P < 0.003) in a mean molar ratio of 1:19, similar tothat reported in other birds. In the larger dowitcherspecies, we also examined exposure to 20organochlorine compounds. Organic analyses showedthat the dowitchers had been exposed to DDE, PCBs,dieldrin and trans-nonachlor, but with no significantdifferences in concentrations between Hayward andNewark (P > 0.05).     

土壤和底泥中砷、铬、锰测定的前处理技术

试验了土壤和底泥中砷的前处理技术,其目的是能对土壤、底泥中砷、铬、锰在一次前处理中制备成试液,比色法分析。试验表明,用Ｈ２ＳＯ４－Ｈ３ＰＯ４－Ｈ２Ｏ２进行前处理是可行的。方法简单、挥发酸雾少,用标准参考物质检验证明,分解完全,数据准确,有粒较好一致性。     

Hydrologic–Economic Model for Managing Irrigation Intensity in Irrigation Areas under Watertable and Soil Salinity Targets

This paper gives mathematical details and sample applications of SWAGMAN Farm (SWAGMAN, Salt Water and Groundwater Management), a farm-scale hydrologic economic model that integrates agronomic, climatic, irrigation, hydrogeological and economic aspects of irrigated agriculture. The model is capable of determining optimum mix of land use to keep watertable and soil salinity within acceptable limits while maximising the economic returns. Alternatively, the model can simulate water and salt balance and economics of a given cropping preference. Web-based and Geographic Information Systems versions of the model are available for integration with the environmental reporting systems of the irrigation areas.     

Cyanobacterial Flora from Polluted Marine Shores

Citation of cyanobacterial cultures from the shores of south west coast of Gujarat, India and their relationship with sea water quality, influenced by extensive pollutant runoff is reported in this study. Intensity of pollution was evaluated by physico-chemical analysis of water. Higher load of suspended solids (60–1000 mg l⁻¹) and nutrients (PO₄ ⁻P: 1.3–4 μmole l⁻¹ and NO₃ ⁻N: 12.5–17.8 μmole l⁻¹) were persistent throughout the analysis. Community structure is seen to be influenced by such persistent pollution. Twenty nine cyanobacterial species were isolated belonging to 9 genera of 4 families, with an elevated occurrence of Oscillatoria and Lyngbya species. No heterocystous cyanobacteria were isolated throughout the study.