直接进样-超高效液相色谱-串联质谱测地表水中丙烯酰胺

建立了超高效液相色谱-串联质谱测定地表水中丙烯酰胺的分析方法。水样经0.22μm微孔滤膜过滤,直接进样,通过多反应监测(71.8→54.9)定性,外标法定量,方法的检出限为0.1μg/L,回收率为97.8%~98.7%,6次测定值相对标准偏差小于7.0%,为地表水中丙烯酰胺的监测提供了一种快速、准确、灵敏的分析方法。     

超高效液相色谱-串联质谱同时测定水中的敌百虫和敌敌畏

建立超高效液相色谱-串联质谱(UPLC-MS-MS)同时测定水中敌百虫和敌敌畏的方法。水样经0.22μm滤膜过滤,直接用超高效液相色谱-三重四极杆串联质谱多级反应监测法(MRM)定量检测敌百虫、敌敌畏。考察了色谱柱、流动相、滤材对分析的影响,并确定了最佳分析条件。最佳条件下,敌百虫、敌敌畏的检出限分别为0.6μg/L和2.3 ng/L。用建立的方法测定了4种实际水样中的敌百虫、敌敌畏,水样加标回收率为82.2%~112.1%。方法简便快捷、绿色环保,适合于地表水及地下水中敌百虫和敌敌畏的同时分析。     

SPE-HPLC法测定水中硝基苯酚类化合物

建立了以固相萃取为前处理条件,用液相色谱法测定水中10种硝基苯酚类化合物的分析方法。实验使用HLB(6 L/150 g)固相萃取柱富集水样中的目标化合物,二氯甲烷与乙酸乙酯体积比1:2的混合溶剂洗脱,采用Phenyl柱(4.6 mm×250 mm,5 μm)分离目标化合物,以乙腈(1%甲酸)/水(1%甲酸)为流动相进行梯度洗脱,二极管阵列检测器检测。10种硝基苯酚类物质在0.02~10 mg/L范围内呈现良好的线性。方法检出限为0.1~0.3 μg/L,水样加标相对标准偏差为5.19%~18.2%,平均加标回收率为49.8%~124%。该方法适用于水中10种硝基苯酚类化合物的测定。     

超高效液相色谱—三重四级杆质谱法测定水中红霉素

应用超高效液相色谱—三重四极杆质谱联用仪(UPLC-MS/MS)建立了地表水、地下水、工业废水中红霉素的分析方法。通过对淋洗液、色谱流动相等进行优化,确定以直接进样、乙腈为淋洗液、水(0.1%甲酸)—乙腈为流动相进行水样预处理和色谱分离。在最优条件下,目标物在水中的回收率为95.4%～114%,相对标准偏差(RSD)为1.2%～9.0%。目标物化合物的线性范围为0.01～50.0μg/L,线性相关系数(R~2)不小于0.998。该方法具有检出限低、回收率高等优点,经实际样品测试,适用于水中红霉素的检测。     

乙腈盐析萃取HPLC-PDA同时测定水中11种苯胺类化合物

通过对色谱分析和样品萃取条件的选择和优化，建立了同时分析水中11种苯胺类化合物的HPLC方法。样品经乙腈盐析萃取后直接进样分析，采用 ODS色谱柱，以乙腈-水为流动相进行梯度洗脱，用PDA检测。结果表明，11种苯胺类化合物在0.20~100mg/L范围内其浓度和检测信号呈良好的线性关系，方法检出限为0.002~0.007mg/L，地表水和废水样品加标回收率为81.6%~97.4%，相对标准偏差为1.5%~5.5%。     

超高效液相色谱三重四极杆质谱联用法测定水中的丙烯酰胺

将含有丙烯酰胺的水样过滤后加入甲酸酸化,然后直接进样,使用超高效液相色谱三重四极杆质谱联用法测定,通过选择离子反应监测,可实现定性和外标法定量分析.该方法测定生活饮用水及其水源水中丙烯酰胺的最低检测浓度为0.15 g/L,对实际样品的加标回收率在92％ ～ 123％,该方法绿色环保、简单方便,且具有较高的灵敏度和较低的检出限.     

直接进样-高效液相色谱-串联质谱分析水中微囊藻毒素

建立了直接进样-高效液相色谱-串联四极杆质谱分析环境水样中微囊藻毒素-LR的分析方法。方法使用C18反相柱为分离柱,柱温40℃,流速0.7 mL/min,乙腈和甲酸水溶液(0.1%)作流动相,采用梯度洗脱,保留时间4.13 min。串联质谱采用多反应监测模式,使用ESI(+)源电离水样。在上述条件下,水样过粒径为0.45μm的滤头后可直接进样,进样体积25μL时检出限可达0.04μg/L,在0.10~200μg/L范围内线性良好(R=0.999 8);样品加标回收率为96.6%~106%,相对标准偏差为1.3%~5.6%。同时方法应用到实际环境水样分析中也具有令人满意的结果。该方法灵敏度高,快速简单,适用于环境水样中MC-LR的分析。     

超高效液相色谱-串联质谱法测定水中拟除虫菊酯和有机磷农药残留

采用直接进样法和萃取浓缩法2种前处理方式,通过超高效液相色谱-串联质谱法对水中20种拟除虫菊酯类和有机磷类农药进行了测定,并对仪器条件的选择和前处理条件的优化进行了探讨。结果表明,20种农药的线性关系良好,相关系数均>0.999,直接进样法检出限为0.21~2.47μg/L,回收率为81.0%~119%,相对标准偏差<10%。萃取浓缩法检出限为0.0022~0.0043μg/L,回收率为71.5%~115%,相对标准偏差<15%。该方法简便、快捷,精密度和准确度较高,可满足水中拟除虫菊酯类和有机磷类农药的检测要求。     

气相色谱法测定水中的苦味酸

建立了毛细管柱气相色谱-微池电子捕获检测器测定水中苦味酸的方法。水样中的苦味酸经次氯酸钠氯化衍生后,经正己烷提取后进行气相色谱分析。考察了萃取溶剂和次氯酸钠加入量对萃取的影响。在优化萃取条件下,苦味酸在25~500μg/L范围内有良好的线性关系。在低、中、高三个添加水平,苦味酸的回收率为83.0%~91.74%,相对标准偏差为1.79%~3.82%。     

GC-C-IRMS测定污染场地土壤中苯系物单体碳同位素比值

选取苯系物中的代表性组分苯、甲苯和二甲苯等化合物,通过热脱附、气相色谱质谱条件的优化及方法学考察,建立了热脱附进样-气相色谱-同位素比值质谱(GC-C-IRMS)测定苯系物单体碳同位素比值的方法。结果表明,单体化合物进样量在0.3μg以上均能满足测定要求;与直接进样方式相比,热脱附进样对单体碳同位素比值测定无分馏影响;标准溶液和苯系物土壤样品测定结果的RSD分别为1.0%~1.7%和0.3%~2.6%。     

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.     

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 %.     

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.     

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。     

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.     

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。     

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。