通过式固相萃取/超高效液相色谱-串联质谱法测定蔬菜中18种农药残留

建立了超高效液相色谱-串联质谱(UPLC-MS;MS)快速测定蔬菜中18种农药残留的方法.样品经乙腈提取后,经Oasis PRiME HLB固相萃取柱净化,采用ACQUITY UPLC HSS T3 C18(50 mm×2.1 mm,1.8μm)色谱柱进行分离,以0.1%甲酸水溶液和乙腈作为流动相进行梯度洗脱.采用电喷雾电离源、正离子模式下以多反应监测(MRM)进行定性和定量分析.结果表明,18种农药在0.5—50μg·L^-1范围内线性关系良好(r2>0.995),方法最低检出限为0.4—1.5μg·kg^-1,最低定量限为1.4—5.0μg·kg^-1.在韭菜、芹菜、番茄、白菜基质中,5、10、50μg·kg^-1添加水平下的加标回收率为60.2%—126.9%,相对标准偏差(RSD)为0.4%—21.6%(n=3).     

纸喷雾离子源质谱对易燃液体的快速分析方法研究

为提高对易燃液体的快速检测分析能力,在经典纸喷雾质谱的基础上,发展建立了三种新型的基于纸喷雾离子化的质谱方法,分别为基于针尖辅助纸喷雾质谱、基于导电纸辅助纸喷雾质谱、基于金属网辅助纸喷雾质谱。结果显示,在优化的实验条件下,可以迅速检测到样品中的目标化合物质子化峰。对于汽油样品,目标化合物主要是烷基吡啶类同系物;对于柴油样品,目标化合物主要是几种系列的含氮杂环芳香族化合物的同系物。对汽油和柴油样品的检测浓度均能达到5×103 ppm。这三种敞开式离子源质谱方法在对易燃液体的分析中,具有选择性好、无需样品前处理、分析迅速的特点。     

包埋固定化硝化污泥处理氨氮废水的过程特性

采用聚乙烯醇（PVA）包埋硝化效能良好的活性污泥制备固定化颗粒,针对不同初始氨氮浓度的模拟废水,基于序批式间歇反应器小试实验,探讨了包埋颗粒的传质效能与氮去除过程特性.实验结果表明：颗粒体积投加率为10%,实验水温为26~30℃,pH值为7.5~8.5,反应器DO浓度为4~5mg/L的条件下,各初始氨氮浓度（50~400mg/L）稳定期包埋颗粒最大氨氮去除负荷为61.8~242.3mgN/（L-particles·h）.包埋颗粒对氨氮的去除较符合零级反应动力学模型,其最大氨氧化速率（μ_max）为271.40mgN/（L-particles·h）,半饱和常数K_s为66.69mg/L,包埋颗粒内氨和氧的有效扩散系数（D_e）分别为0.467×10^-9m²/s、0.279×10^-9m²/s.SEM观察和比表面积测试结果表明,与新鲜颗粒相比,稳定期颗粒内部的比表面积和平均孔径增加.包埋颗粒,活性污泥,包埋颗粒与活性污泥混合3种体系对比实验表明,各初始氨氮浓度条件下混合体系可显著强化生物硝化与脱氮过程,并发生同时硝化反硝化现象.     

气相色谱-三重四级杆质谱测定环境样品中17种二 英

研究了基于Agilent气相色谱-三重四级杆质谱测定环境样品中17种二 英的分析方法.结果表明,在浓度范围0.5~2000ng/mL之间具有良好的线性,17种二 英的相对响应因子在0.96~1.21之间,相对标准偏差< 14%,定量限范围在0.080~2.83pg/μL之间,适合环境样品中超痕量二 英的分析.利用该方法对第15轮二 英国际实验室比对的沉积物样品进行了测试,总I-TEQ值落在Intercal给定的中位值±标准偏差范围内.研究选取污染源烟道气、飞灰、土壤和沉积物等40多个环境样品进行测试,并与高分辨质谱测定结果比较表明,当环境样品中二 英浓度在0~60ng I-TEQ范围,两者数据具有较好的线性相关性,R2=0.997.就17种单体而言,利用三重四级杆质谱测定的2,3,7,8-TCDF和1,2,3,7,8,9-HxCDF结果会高于高分辨质谱,而1,2,3,7,8,9-HxCDD的结果低于高分辨质谱的测定值.鉴于三重四级杆质谱在购置、维护和能耗等方面的低成本优势,本方法可作为简易经济的环境中超痕量二 英的分析方法.     

Single particle analysis of ambient aerosols in Shanghai during the World Exposition, 2010: two case studies

ATSI Model 3800 aerosol time-of-flight mass spectrometer (ATOFMS) was deployed for single-particle analysis in Shanghai during the World Exposition (EXPO), 2010. Measurements on two extreme cases: polluted day (1st May) and clean day (25th September) were compared to show how meteorological conditions affected the concentration and composition of ambient aerosols. Mass spectra of 90496 and 50407 particles were analyzed respectively during the two sampling periods. The ART-2a neural network algorithm was applied to sort the collected particles. Seven major classes of particles were obtained: dust, sea salt, industrial, biomass burning, organic carbon (OC), elementary carbon (EC), and NH₄-rich particles. Number concentration of ambient aerosols showed a strong anti-correlation with the boundary layer height variation. The external mixing states of aerosols were quite different during two sampling periods because of different air parcel trajectories. Number fraction of biomass burning particles (43.3%) during polluted episode was much higher than that (21.6%) of clean time. Air parcels from the East China Sea on clean day diluted local pollutant concentration and increased the portion of sea salt particle dramatically (13.3%). The large contribution of biomass burning particles in both cases might be an indication of a constant regional background of biomass burning emission. Mass spectrum analysis showed that chemical compositions and internal mixing states of almost all the particle types were more complicate during polluted episode compared with those observed in clean time. Strong nitrate signals in the mass spectra suggested that most of the particles collected on polluted day had gone through some aging processes before reaching the sampling site.     

Assessment of potentially toxic elements in Swiss chard and sediments of Akaki River,Ethiopia

For the determination of 15 potentially toxic elements (V, Cr, Fe, Mn, Co, Ni, Cu, Zn, As, Se, Ag, Cd, Sn, Hg, and Pb) in plant and sediment samples of the Akaki River, Ethiopia, inductively coupled plasma–mass spectrometry, inductively coupled plasma–optical emission spectrometry, and a RA-915+ mercury analyzer were applied. Sediment and plant samples were mineralized using a closed-vessel microwave-assisted digestion system. The elemental concentrations varied considerably in plant and sediment samples. The minimum concentration was observed for known toxic elements (As, Hg, and Cd) while the highest concentration was observed for the elements of relatively low toxicity Zn, Mn, and Fe. The concentration of Cr, Fe, Pb, Zn, and As in Swiss chard surpassed the maximum permissible levels at specific sites. At some of the sites, the sediment quality guidelines are surpassed for Cu, Zn, and Pb.     

Occupational exposure to airborne aromatic amines in rubber manufacturing: Determination by gas chromatography‐mass spectrometry

Aromatic amines (AAs) are used in a variety of chemical industries and consequently they are the object of great attention in occupational hygiene owing to the carcinogenic effects that many of them have shown. This work outlines a procedure for the determination of occupational exposure to airborne AAs in the rubber industry and the application of this method in a tyre manufacturing plant using p‐phenylenediamines as antiozonants. Samples were collected on a glass fibre filter followed by a silica gel tube and analyzed by GC‐MS/SIM using a capillary column coated with methyl silicone. p‐Phenylendiamines and other AAs probably formed as thermodegradation products were found in concentrations of up to 10 μg/m³ during rubber vulcanization.     

Source and material balance of total organic halogen pollution in the Ayase River system,Japan

The total organic halogen (TOX) pollution in the highly polluted Ayase River system was investigated. Using the concentration of coexisting linear undecylbenzenesulfonate and the difference in the flowing water volume between summer and winter, the fractions of domestic and agricultural wastewaters in the whole water column were calculated and the variety of the TOX sources in the river was estimated. The river carried about 100 kgCl of TOX materials in one day; about 50 kgCl of the materials was from residential area in the basin. The contribution of agricultural drainage from paddy field was not negligible in summer. Highly contribution of industrial wastewater was observed in a tributary Furuayase River basin while the amount of TOX loaded in the area was widely varied; 0–105 kgCl of the materials was discharged as industrial wastewater.     

Physicochemical properties of non-living water hyacinth (Eichhornia crassipes) and lesser duckweed (Lemna minor) and their influence on the As(V) adsorption processes

Eichhornia crassipes (Ec) and Lemna minor (Lm) are aquatic plants. They are considered as weeds of the water and approach being a scourge in many parts of the world, choking waterways and hindering transport upon them. At the same time they are known to readily remove heavy metal ions from water. This paper considers the use of non-living plants as novel and inexpensive biosorbent for the removal of As(V) from watersheds. In the first place they were conditioned and characterised to determine their physicochemical and surface properties and in the second place their adsorption properties for As(V) from aqueous solution were evaluated considering the toxicity of this metalloid in the environment. It describes the methodology to prepare the non-living biomasses; the physicochemical characterisation by SEM, XRD, FTIR, TGA analyses and surface characterisation of Ec and Lm by specific surface, hydration kinetic, point of zero charge determination by mass titration, active site density and XPS analysis are described. Both studied biomasses were found to be potential bio-sorbents for arsenic ions from aqueous solution. According to their efficiency to remove arsenic, they can be used in a very low cost metalloid ions removal system.     

超高效液相色谱串联质谱法检测鱼体中的全氟化合物

采用超高效液相色谱-串联质谱联用法(UPLC-ESI-MS/MS),建立了检测1种贝类和2种鱼类的肌肉组织中11种全氟化合物(PFCs)的分析方法.采用碱液消解做为样品前处理法,选Carbon/NH2双层SPE小柱做为净化小柱,并以ACQUITY UPLC BEH C18为分析柱,甲醇和2 mmol.L-15%甲醇乙酸铵溶液为梯度淋洗液.所选定的11种全氟化合物在6 min内就可以达到良好分离,外标法定量.平均回收率在72.1%—93.6%之间,相对标准偏差在0.6%—9.5%之间,实际检出限在3.4—26.7 pg.g-1.