Method optimization to measure polybrominated diphenyl ether (PBDE) concentrations in soils of Bratislava, Slovakia

We modified an analytical method to determine polybrominated diphenyl ethers (PBDEs) in urban soils of Bratislava (Slovakia). Gel permeation chromatography (GPC) introduced as a clean-up step for soil extracts substantially reduced matrix enhancements when PBDEs were measured with gas chromatography-negative chemical ionization-mass spectrometry (GC-NCI-MS). The resulting method proved to be accurate, precise, and showed low detection limits. The sum of 15 PBDE concentrations in surface horizons of Bratislava soils ranged from 87 to 627 pg g⁻¹. PBDE concentrations were mostly higher in surface than deeper horizons probably because of atmospheric deposition and lack of substantial vertical transport. Lower brominated PBDEs undergo more soil-atmosphere exchanges or are more scavenged and transferred with litter fall to the soil organic matter than higher brominated ones as suggested by the correlation between lower brominated PBDEs and soil organic C (C_org) concentrations.     

葡多酚对口服乙醇小鼠肝细胞PCNA和Bcl-2表达的影响

为观察葡多酚(GPC)对小鼠乙醇性肝损伤的防护作用,将每天经口灌胃给予4 g·(kg·bw)-1乙醇的小鼠同时分别给予不同剂量的GPC,30 d后处死小鼠;取肝组织用MTT法检测各组小鼠肝细胞的增殖活性,用免疫组化法和图像分析方法检测PCNA和Bcl-2表达水平.结果显示:GPC高剂量组16 h的肝细胞增殖活性为0.4...     

全自动凝胶色谱净化-气相色谱法同时测定淡水鱼类中多氯联苯和有机氯农药等36种残留有机物

建立了淡水鱼类中多氯联苯和有机氯农药等36种半挥发性有机物的同时测定方法。样品用正己烷和丙酮(体积比为1∶ 1)进行提取,提取溶液经凝胶色谱和弗罗里硅土两级净化,浓缩后采用气相色谱法测定,回收率为70.3%~84.8%,检出限为0.05~0.20ng/g。该方法准确度和回收率较好,适合淡水鱼类中多氯联苯和有机氯农药含量的测定。     

Method for the determination of selected organochlorine pesticides and polychlorinated biphenyls in human serum based on a gel permeation chromatographic clean-up

A gel permeation chromatographic (GPC) clean-up based method was developed for determination of selected organochlorine pesticides and polychlorinated biphenyls in human serum. The method permits automation of the sample extract clean-up stage and is designed to work with small amounts of sample. Different working variables were studied in its development, including injection volume, flow rate, and fat amount as the most representative coextract. The method provides solvent and time savings. Initial extraction was performed using 96-well solid-phase disk extraction plates, and quantification was performed by gas chromatography with electron capture detection and mass spectrometry. Recoveries of PCB congeners 28, 52, 101, 118, 138, 153, and 180 and organochlorine pesticides HCB, β-HCH, γ-HCH, heptachlor epoxide, p,p′-DDE, and p,p′-DDT at two spiking levels ranged from 55% to 115% with relative standard deviations ranging from 2.0% to 14.6%. Limits of quantification ranged from 0.06 to 0.16 ng mL⁻¹ for PCBs and from 0.12 to 0.36 ng mL⁻¹ for organochlorine pesticides. Finally, the method was applied to the analysis of 38 serum samples and the results were compared with those of another procedure validated at the laboratory.     

加速溶剂萃取/气相色谱质谱法测定鱼类样品中的多环麝香

建立了鱼类样品中5种多环麝香的分析方法.采用加速溶剂萃取(ASE)提取,经凝胶渗透色谱(GPC)以及中性氧化铝层析柱净化后,浓缩并定容洗脱液,用GC-SIM-MS进行检测.本方法对替代物标样荧蒽-d10.的回收率为92.7%-112.9%.以六氯苯(13C)为内标,5种合成麝香的线性范围为1.0-1000.0 ng·g...     

Degradation of Commercial Biodegradable Packages under Real Composting and Ambient Exposure Conditions

The use of long-lasting polymers as packaging materials for short lived applications is not entirely justified. Plastic packaging materials are often soiled due to foodstuffs and other biological substances, making physical recycling of these materials impractical and normally unwanted. Hence, there is an increasing demand for biodegradable packaging materials which could be easily renewable. Use of biopolymer based packaging materials allows consideration of eliminating issues such as landfilling, sorting and reprocessing through taking advantage of their unique functionality, that is compostability. Composting allows disposal of biodegradable packages and is not as energy intensive compared to sorting and reprocessing for recycling, although it requires more energy than landfilling. The aim of this work was to study the degradation of three commercially available biodegradable packages made of poly (ld-lactide) (PLA) under real compost conditions and under ambient exposure by visual inspection, gel permeation chromatography, differential scanning calorimetry, and thermal gravimetric analysis. A novel technique to study the degradability of these packages and to track the degradation rate under real compost conditions was used. The packages were subjected to composting for 30 days, and the degradation of the physical properties was measured at 1, 2, 4, 6, 9, 15 and 30 days. PLA packages made of 96% l-lactide exhibited lower degradation than PLA packages made of 94% l-lactide, mainly due to their highly ordered structure, therefore, higher crystallinity. The degradation rate changed as the initial crystallinity and the l-lactide content of the packages varied. Temperature, relative humidity, and pH of the compost pile played an important role in the total degradation of the packages. A first order degradation of the molecular weight as a function of time was observed for the three packages.     

溢油的GPC色谱鉴定

本文利用ＧＰＣ色谱测定物质分子量分布的特点，对溢油和怀疑溢油源ＧＰＣ色谱测定的结果，进行比较，找出溢油源。     

加速溶剂萃取/凝胶渗透色谱净化/气相色谱-负化学离子源质谱测定生物样品中的四溴联苯醚

建立了一种分析生物样品中四溴联苯醚（BDE-47）的方法.获得了优化的前处理条件和GC/MS检测条件,采用加速溶剂萃取（ASE）-凝胶渗透色谱（GPC）/多层硅胶-氧化铝复合柱净化,气相色谱-质谱（负化学离子源）（GC/NCI-MS）分析.以猪肝为基质的BDE-47加标回收率结果为77.3%—118.7%,相对标准偏差...     

快速溶剂萃取—凝胶渗透色谱净化-GC／MS分析土壤中酞酸酯（PAEs）

采用毛细管柱气相色谱-质谱选择离子检测技术，结合加速溶剂萃取和凝胶渗透色谱净化方法，分析土壤中的6种酞酸酯类（PAFs）化合物。结果表明，土壤中6种PAEs检出限在14—42μg/kg间，加标平均回收率为65．5％～104．4％，相对标准偏差为5．19％～9．61％。方法具有操作简便、纯化效果好和对环境友好的特点，且具有很强的实用性。     

鳊肌肉中有机磷农药GPC净化条件的选择

为了确定鳊肌肉中乐果、甲基对硫磷、马拉硫磷3种有机磷农药GPC(凝胶渗透色谱)的最佳净化条件,运用“完全随机设计2因素折因设计”编辑不同的GPC单浓缩方法,通过气相色谱仪测定浓缩后农药溶液的浓度.比较样品浓度的标准偏差来确定GPC和气相色谱的精密度.比较有机磷农药加标回收率,用SPSS 16.0统计软件中的广义线性模型进行方差分析,确定适宜浓缩条件.通过持续分段收集法确定有机磷农药的适宜收集时间.采用确定的适宜收集时间和单浓缩条件对鳊肌肉中提取的有机磷农药进行净化.结果表明,在0.01～ 1.0 mg/L范围内3种农药组分含量与峰面积呈线性相关(相关系数为0.997～0.998).乐果、甲基对硫磷、马拉硫磷的定性检出限分别为7.27 ng/ks、7.15 ng/kg、7.15 ng/ks,定量检出限分别为40.3ng/kg、37.3 ng/kg、38.0ng/kg.GPC净化的适宜条件:以环己烷:乙酸乙酯=1:1(体积比)为溶剂;柱流速为5.0 mL/min;定量进样环进样量为5.0 mL;除杂质时间为1 080s,收集目标物时间为480 s,洗柱时间为300 s;浓缩温度为40℃;第1阶段真空泵压力为18 000 Pa或19000Pa,第2阶段真空泵压力为20 000 Pa或21 000 Pa.适宜净化条件下乐果、甲基对硫磷、马拉硫磷的回收率为83.59％～ 95.19％.在气相色谱仪和GPC精密度较好、标准工作曲线良好的情况下,确定了GPC对鳊肌肉中3种有机磷农药的适宜净化条件,回收率较好,检出限低于国家标准,符合淡水鱼类中有机磷农药的检测要求.