固相萃取-高效液相色谱法测定武汉东湖水体中微囊藻毒素

建立了固相萃取-高效液相色谱法(SPE-HPLC)测定东湖水样中微囊藻毒素(MC)的方法,考察了不同流动相、淋洗液和洗脱液对MC-RR和MC-LR测定的影响。结果表明,MC-RR和MC-LR的方法检出限分别为0.0789μg/L和0.0234μg/L,其线性定量范围分别为0.1～10.0mg/L和0.06～10.0mg/L;样品测定回收率为78.4%～97.4%,RSD小于6.3%。该法灵敏度高,快速准确,用于实际水样测定的结果令人满意。     

UPLC-MS/MS测定地表水中总微囊藻毒素的快速前处理方法探究

为方便地表水中总微囊藻毒素(TMCs)的预警监测,探究提取MC-LR、MC-RR、MC-YR的不同快速前处理方法,建立同时测定3种TMCs的煮沸-过滤-UPLC-MS/MS法。该方法在0.006μg/L~50.0μg/L范围内线性良好,方法检出限为0.006μg/L~0.010μg/L,实际水样3个质量浓度水平的加标回收率为88.6%~108%,6次测定结果的RSD为2.6%~9.4%。     

响应面法优化测定水体中微囊藻毒素

针对水体中低浓度微囊藻毒素(MC-RR和MC-LR)的富集、淋洗、洗脱等前处理环节,采用单因素响应面优化法探讨微囊藻毒素前处理的最佳条件。结果表明:采用体积分数为25%的甲醇水溶液能够取得最佳淋洗效果,由One Factor设计优化得到体积分数为75%的甲醇水溶液作洗脱剂,MC-RR和MC-LR最佳回收率为89.4%和90.7%。方法在0.100 mg/L~5.00 mg/L范围内线性良好,MC-RR和MC-LR的检出限分别为0.07μg/L和0.04μg/L,实际水样加标回收率分别为80.6%和84.9%,平行测定结果的RSD分别为1.6%和2.4%。     

水中3种微囊藻毒素的高效液相色谱测定方法优化

对天然水体中3种痕量微囊藻毒素（MC-RR、MC-YR、MC-LR）的淋洗、洗脱、液相色谱测定等环节进行单因素不同水平考察,结果表明：以体积分数为45%的甲醇水溶液（含0.1%的TFA）为固相萃取淋洗剂、10 mL甲醇（含01%TFA）为固相萃取洗脱剂,体积分数为70%的甲醇水溶液（含0.1%TFA）为液相色谱流动相,可在6 min内有效分离MC-RR、MC-YR、MC-LR。将优化后的方法用于实际加标水样的测定,MC-RR、MC-YR、MC-LR的方法检出限分别为0.064 μg/L、0.098 μg/L、0.095 μg/L,加标回收率为87.0%~116%,RSD为10.2%~18.8%。     

超高效液相色谱/串联质谱法测定饮用水源水中多种藻毒素

饮用水源水样品经过直接进样或固相微萃取法净化后,用超高效液相色谱/串联质谱测定水中11种藻毒素。通过试验优化测定条件,使该方法在0.500μg/L~50.0μg/L范围内线性良好,检出限为0.01μg/L~0.05μg/L。对同一实际环境样品做3个质量浓度水平加标回收试验,6次测定结果的RSD为2.2%~9.3%,回收率为76.1%~108%。将该方法用于测定环巢湖湖面12个监测断面水样,结果 3组样品中MC-YR、MC-LR和MC-RR值为0.3μg/L~0.8μg/L。     

HPLC-高分辨飞行时间质谱测定水中多种微囊藻毒素

水样经HLB小柱富集、净化后，采用高效液相色谱-四极杆-高分辨飞行时间质谱同时测定水样中MC-LA、MC-LF、〖JP3〗MC-LR、MC-LW、MC-LY、MC-RR、MC-YR、MC-WR等8种微囊藻毒素。试验表明，8种微囊藻毒素在0500 μg/L～〖JP〗100 μg/L范围内线性良好，方法检出限为0001 μg/L～0005 μg/L，自来水空白样品3个质量浓度水平的加标回收率为725%～998%，5次测定结果的RSD为19%～112%。将该方法用于测定珠海本地水产养殖鱼塘和小型水库的水样，结果均未检出     

宁波市饮用水源地爆发蓝藻水华时微囊藻毒素的污染分析

通过固相萃取净化,建立了超高效液相色谱-串联四极杆质谱法测定水中微囊藻毒素MC-LR和MC-RR的方法,并用该方法监测了宁波市两个饮用水源地爆发蓝藻水华时水体中的微囊藻毒素.监测结果表明,姚江水体中的微囊藻毒素污染水平低,MC-LR和MC-RR没有被检出;梅湖水库水体中MC-RR也未被检出,采取措施后,虽MC-LR有时被检出,但最高时也低于国家标准值(1.0μg/L).     

原子荧光光谱法同时测定环境水体中痕量锡和锌

采用原子荧光光谱法同时测定环境水样中痕量锡和锌,优化了试验条件。锡在1.00μg/L～10.0μg/L、锌在20.0μg/L～200μg/L范围内线性良好,方法检出限锡为0.13μg/L,锌为1.76μg/L,锡和锌标准溶液测定的相对标准偏差分别为2.9%和4.0%,环境水样加标回收率锡为96.4%～106%,锌为92.0%～111%。     

UPLC-MS/MS法同时测定地表水中多种药物及个人护理品

采用快速液相色谱-三重四级杆串联质谱仪(UPLC-MS/MS)测定地表水中31种药物及个人护理品,通过优化分析条件,使方法在0.01μg/L～10.0μg/L范围内线性良好,方法检出限为0.2 ng/L～1.2 ng/L。地表水样品两个质量浓度水平的加标回收率为64.8%～125%,测定6次结果的RSD≤11%。将该方法用于上海市两条河道中10个水样的测定,结果地西泮、氟康唑、甘宝素、咖啡因、可替宁、氨基比林的测定值为6.56 ng/L～302 ng/L,其余PPCPs未检出。     

超高效液相色谱-电喷雾串联四级杆质谱法快速分析水中微囊藻毒素LR

建立超高效液相色谱-电喷雾串联四极杆质谱快速测定水中微囊藻毒素LR(MC-LR)的方法。水样经0.2μmGHP一次性针头过滤器过滤,应用超高效液相色谱/电喷雾串联四极杆质谱仪多离子反应监测(MRM)法定量检测MC-LR。经方法学验证,该方法对MC-LR的最低检出限LOD为0.08μg/L(进样量10μl),最低定量限LOQ是0.10μg/L。在0.2~20.0μg/L的线性范围中,相关系数r=0.9982,回收率范围91.5%~110.3%。方法灵敏度高,专属性强,操作简便快速,定量准确,测定浓度范围宽,是环境水质样品中MC-LR含量检测的理想方法。     

河流沉积物中有机污染物的分析研究进展

总结了近年来河流沉积物中有机污染物的研究进展 ,集中评述了国内有关沉积物中多环芳烃、有机氯农药和多氯联苯的分析研究现状 ,包括样品采集、样品前处理和样品分析 ,并对今后河流、湖泊及水库沉积物中污染物的分析工作作了展望     

Trends in Nitrogen Transport in Swedish Rivers

Concern about nitrogen loads in marine environments has drawn attention to the existence and possible causes of long-term trends in nitrogen transport in rivers. The present study was based on data from the Swedish environmental monitoring programme for surface water quality; the continuity of these data is internationally unique. A recently developed semiparametric method was employed to study the development of relationships between runoff and river transport of nitrogen since 1971; the observed relationships were then used to produce time series of flow-normalised transports for 66 sites in 39 river basins. Subsequent statistical analyses of flow-normalised data revealed only few significant downward trends (p 0.05) during the time period 1971–1994, and the most pronounced of these downward trends were caused by reduced point emissions of nitrogen. The number of significant upward trends was substantially larger (15 for total-N and 18 for NO₃-N). Closer examination of obtained results revealed the following: (i) the most pronounced upward trends were present downstream of lakes, and (ii) observed increases in nitrogen transport coincided in time and space with reduced point emissions of phosphorus or organic matter. This indicated that changes in the retention of nitrogen in lakes were responsible for the upward nitrogen trends. The hypothesis that nitrogen saturation of forest soils has caused a general increase in the riverine export of nitrogen from forested catchments in Sweden was not confirmed. Neither did the results indicate that improved agricultural practices have reduced the export of nitrogen from agricultural catchments.     

Fluoride in groundwater in selected villages in Eritrea (North East Africa)

A study was undertaken to estimate fluoride content in thegroundwater in certain parts of rural Eritrea, North-East Africa,along the River Anseba. Standard procedure was adopted for fluoride detection. Results indicate elevated concentration offluoride in groundwater. The highest concentration was found tobe 3.73 mg L^-1, well above the safety level for consumption.Geological basis for the high concentration of high fluoride hasbeen established; it is presumed to be the pegmatite intrusion hosted by a granitic batholith. Extensive dental fluorosis has been observed in the population exposed to drinking water of highfluoride content.     

HPLC法测定饲料中维生素A、维生素D 3 和维生素E

建立了以w(C2H5OH)=95 %乙醇直接提取,高效液相色谱仪在波长280 nm和254 nm处连续测定饲料中维生素A、维生素D3和维生素E的方法.色谱柱为大连依利特Hypersil ODS C18(25 cm×4.6 mm×5 μm),流动相为甲醇-水,流速为1.2 mL/min.维生素A、维生素D3、维生素E的质量浓度分别在1.0 mg/L～20.0 mg/L、0.5 mg/L～15.0 mg/L 、2.5 mg/L～50.0 mg/L范围内与峰面积呈良好的线性关系,检测限分别为0.3×10-6 μg、0.04×10-6 μg、5.0×10-6 μg,相对标准偏差分别为1.6 %、2.7 %、2.4 %,平均回收率分别为99 %、102 %、98 %.     

丽水市空气中Pb污染调查

为调查丽水市空气中Pb污染现状，在机动车相对集中的市区布设5个测点，测点高度1．2m；监测周期为1a，每星期采样1d或2d，每天采集1个样，每次采样6h；监测项目为TSP、Pb；评价标准采用GB3095—1996《环境空气质量标准》。结果表明，丽水市各测点空气中Pb最大的季均值、年均值均未超标；常规测点和交通路口测点之间TSP、Pb质量浓度值均存在显著的差异性。     

Organochlorines and Mercury in Waterfowl Harvested in Canada

Samples of breast muscle from 32 species of waterfowl collected from 123 sites across Canada were analyzed for chlorobenzenes (CBz), chlordane-related compounds (CHL), hexachlorocyclohexanes (HCH), DDT, mirex, dieldrin, PCBs and mercury. ΣDDT, ΣCBz and ΣPCB were the compounds most frequently found above trace levels. ΣHCH and ΣMirex were detected the least often. Mercury was detected in all of the mergansers, over 50% of dabbling, bay and sea ducks, and in less than 2% of the geese analysed. The highest levels of contaminants were generally found in birds feeding at higher trophic levels such as sea ducks and mergansers. With the exception of a few samples of mergansers and long-tailed ducks from eastern Canada, which contained ΣPCB concentrations of 1.0–2.4 mg kg⁻¹, ΣPCB levels were less than 1 mg kg⁻¹ wet weight. Only one merganser from eastern Canada had a ΣDDT concentration (2.6 mg kg⁻¹ ww) which was greater than 1 mg kg⁻¹ ww. The highest ΣCHL (0.10 mg kg⁻¹ ww) was also found in mergansers from eastern Canada. Levels of total mercury in breast muscle were either low (< 1 mg kg⁻¹ ww) or below detection limits with the exception of a few samples of mergansers from eastern Canada which contained mercury concentrations of 1.0–1.5 mg kg⁻¹ ww. Health Canada determined that the organochlorine and mercury levels found in samples of breast muscle of ducks and geese analysed in this study did not pose a health hazard to human consumers and therefore these waterfowl were safe to eat.     

兰州市冬季和春季PM2.5金属元素浓度水平与分布

为了解兰州市大气PM2.5中金属元素的污染水平和分布,于2013年冬季和春季在兰州市区4个在线监测点进行PM2.5样品采集,利用ICP-MS分析金属元素浓度。结果表明,Pb、B元素含量高于200 ng/m3,V、Fe元素含量在100~200 ng/m3,其余元素含量低于100 ng/m3,其中Pb含量最高,平均含量达到373.8 ng/m3.各监测点元素含量在冬季和春季各有不同,整体上是冬季高于春季。金属元素在兰州市区的空间分布与兰州市工业排放和气象因素有关,工业排放为主导因素。     

中国1998年度环境质量状况

对我国１９９８年度的环境空气质量,酸雨,主要流域水质,近岸域海水水质,地下水水位与水质,城市声环境、射环境质量,典型区域生态环境的状况进行了综述了与分析,指出了我国的环境污染问题主要是城市空气污染,地面水体污染和城市噪声污染。     

Characteristic Air Temperature Distributions Observed in Summer and Winter in Urban Area in Japan

The air temperature distributions in August (summer) and December (winter) were measured in an approximately 15 × 15-km urban area in Hyogo Prefecture, Japan, in order to study the spatial distribution of the air temperature and to propose effective measures against the heat island phenomenon. The air temperature was measured mainly by using thermometer shelters installed in an elementary school and a junior high school. The characteristic air temperature distribution depended on the season. The air temperature was higher inland than in the coastal region in August but was higher in the coastal region in December. The air temperature index indicated that the area where higher air temperatures would most likely appear was 5 to 10 km inland from the coast in August and around the coast in December. The seasonal air temperature distribution was presumably due to the strength of solar radiation and anthropogenic exhaust heat.     

天津市空气颗粒物中酞酸酯的分布特征

采用气相色谱-质谱仪(GC-MS)对天津市空气颗粒物中15种酞酸酯(PAEs)夏季和冬季的浓度进行了分析测定,研究了酞酸酯污染水平的季节变化,不同季节酞酸酯的功能区差异,15种酞酸酯在颗粒物中的分布特征,以及DBP和DEHP在夏冬两季中的污染特点,分析了产生上述结果的原因,基本说明了天津市空气颗粒物中酞酸酯的污染状况和特点。