顶空气相色谱法测定食品中甜蜜素含量

采用顶空气相色谱法测定食品中甜蜜素含量,探讨了气液相平衡条件及色谱条件的选择,实验结果表明甜蜜素的标准溶液在0.1-0.4μg/l范围内具有良好的线性关系,回收率为87.5%-101.8%,相对标准偏差为2.6%.     

LC-MS/MS determination of pesticide residues in fruits and vegetables

The aim of the research is to evaluate pesticide residue contamination of fresh and frozen fruits and vegetables, agricultural raw material, purchased from Polish farmers for production of frozen fruits and vegetables, and the estimation of the multiresidue method effectiveness expressed as the proportion of pesticides detected in food samples to the total number of pesticides analyzed by multiresidue methods. A total of 144 samples (of black currants, red currants, raspberries, cherries, strawberries, blackberries, cauliflowers and broccoli) were analyzed using LC-MS/MS method for the determination of 60 pesticides. QuEChERS extraction, matrix-matched calibration and dynamic multiple reaction monitoring method were used. Residues of 15 compounds, mainly fungicides and insecticides, were detected in 46 samples. The percentage of samples with residues above the maximum residue levels (MRL) was 15%, whereas samples with residues below MRL were 17%. A total of 13 samples contained more than one pesticide residue. Pesticide residues were detected most often in samples of black currants (50%), broccoli (36.4%), raspberries (29%) and red currants (21.8%). The most frequently detected pesticides were carbendazim and acetamiprid. The proportion of pesticides detected during our study to the total number of analyzed pesticides amounted to 25%. It was compared to literature findings. For three fourth of multiresidue methods, the proportion was below 50% for methods developed for the analysis of less than 100 pesticides, and below 30% for methods developed for the analysis of more than 100 pesticides. It appears that a lot of efforts and means is lost on pesticides never or rarely detected in examined samples. The workload and cost effectiveness of the development and application of multiresidue methods along with the range of pesticides covered by the method should be carefully and thoroughly considered anytime when a new method or workflow is developed. Including non-targeted screenings in pesticide residue control seems to be an alternative worth considering.     

Highly efficient conversion of sugarcane bagasse pretreated with liquid hot water into ethanol at high solid loading

Liquid hot water (LHW), an environmental-friendly physico-chemical treatment, was applied to pretreat the sugarcane bagasse (SCB). Tween80, a non-ionic surfactant, was used to enhance the enzymatic hydrolysis of the pretreated SCB. It found that 0.125 mL Tween80 /g dry matter could make the maximum increase (33.2%) of the glycan conversion of the LHW-pretreated SCB. A self-designed laboratory facility with a plate-and-frame impeller was applied to conduct batch hydrolysis, fed-batch hydrolysis, and the process of high-temperature (50°C) fed-batch hydrolysis following low-temperature (30°C) simultaneous saccharification and fermentation (SSF) which was adopted to overcome the incompatible optimum temperature of saccharification and fermentation in the SSF process. After hydrolyzing LHW-pretreated SCB for 120 h with commercial cellulase, the total sugar concentration and glycan conversion obtained from fed-batch hydrolysis were 91.6 g/L and 68.3%, respectively, which were 9.7 g/L and 7.3% higher than those obtained from batch hydrolysis. With Saccharomyces cerevisiae Y2034 fermenting under the non-sterile condition, the ethanol production and theoretical yield obtained from the process of SSF after fed-batch hydrolysis were 55.4 g/L and 88.3% for 72h, respectively, which were 15.5 g/L and 24.7% higher than those from separate fed-batch hydrolysis and fermentation. The result of this work was superior to the reported results obtained from the LHW-pretreated SCB.     

臭氧氧化法降解聚氯乙烯离心母液废水中3种有机物

以聚氯乙烯离心母液废水中含量较高的3种有机物(聚乙烯醇、异辛醇和α-甲基苯乙烯)作为目标物,考察臭氧氧化工艺对3种有机物的去除效果,同时考察反应时间、臭氧投加量和初始pH对处理效果的影响。实验结果表明,臭氧氧化处理3种废水的最佳反应时间和臭氧投加量分别为:聚乙烯醇25 min,136 mg/L;异辛醇60min,312 mg/L;α-甲基苯乙烯60 min,32 mg/L。在此条件下,3种有机物的去除率分别为98%、85%和95%。此外,碱性条件有助于臭氧氧化工艺对3种有机物的降解。产物分析结果表明,经臭氧氧化,聚乙烯醇断链后进一步反应生成了草酸单乙酯,异辛醇和α-甲基苯乙烯分别生成了和苯乙酮。     

生物滴滤塔处理氯苯废气的工艺性能

将活性污泥培养及驯化后接种于生物滴滤塔中，挂膜启动后处理模拟氯苯废气（简称氯苯废气），考察了生物滴滤塔在挂膜启动阶段及稳定运行阶段的性能。实验结果表明：接种41 d后生物滴滤塔成功挂膜，此时氯苯去除率稳定在90%以上；生物滴滤塔稳定运行阶段，随着进气中氯苯质量浓度由303.82 mg/m³逐渐增至1 489.05 mg/m³，氯苯去除率从85.1%降至70.1%。处理氯苯废气适宜的工艺条件为：空塔停留时间超过45 s，喷淋液流量31.8 mL/min，氯苯负荷23.97~128.01 g/（m³·h）。生物滴滤塔对喷淋液的酸性环境有较好的适应性，喷淋液pH的变化对氯苯去除率无显著影响。     

黄山景观区域降雨微量元素化学组成及来源

通过分析降水化学成分,探讨黄山景观区域降雨的微量元素化学组成特征及其来源。结果表明,降雨中微量元素含量呈现明显的季节性变化,主要受到降雨量、pH值、风向及溶解有机质等因素影响。来源分析和贡献估算结果表明,降雨中Mn、Cu、Pb、Cd、Ni、Co等元素受燃煤和交通污染排放的影响显著,贡献率均在98%以上;土壤源和人为源对Fe的贡献率分别为76. 9%、23. 1%,对Ti的贡献率为22. 8%、77. 2%; Sr主要受海洋源(28. 3%)和人为源(70. 5%)双重影响。     

Investigation of titanium liquid/gas diffusion layers in proton exchange membrane electrolyzer cells

In a proton exchange membrane electrolyzer cell (PEMEC), liquid/gas diffusion layer (LGDL) is expected to transport electrons, heat, and reactants/products to and from the catalyst layer with minimum voltage, current, thermal, interfacial, and fluidic losses. In addition, carbon materials, which are typically used in PEM fuel cells (PEMFCs), are unsuitable in PEMECs due to the high ohmic potential and highly oxidative environment of the oxygen electrode. In this study, a set of titanium gas diffusion layers with different thicknesses and porosities are designed and examined coupled with the development of a robust titanium bipolar plate. It has been found that the performance of electrolyzer improves along with a decrease in thickness or porosity of the anode LGDL of titanium woven meshes. The ohmic resistance of anode LGDL and contact resistance between anode LGDL and the anode catalyst play dominant roles in electrolyzer performance, and better performance can be obtained by reducing ohmic resistance. Thin titanium LGDLs with straight-through pores and optimal pore morphologies are recommended for the future developments of low-cost LGDLs with minimum ohmic/transport losses.     

高效液相色谱-三重四级杆/复合线性离子阱质谱法测定饮用水中22种邻苯二甲酸酯

建立了一种同时测定饮用水中22种邻苯二甲酸酯(PAEs)的高效液相色谱-三重四级杆/复合线性离子阱质谱方法:饮用水样品经针头过滤器过滤,选用Biphenyl液相色谱柱进行分离,以含0.1%甲酸的水溶液和含0.1%甲酸的甲醇溶液为流动相,电离模式为电喷雾正离子,选用多反应监测触发增强子离子扫描模式进行检测。结果表明,22种PAEs的灵敏度良好,定量限为0.001～0.1 μg/L。配制浓度为0.1～100.0 μg/L的混标溶液进行进样分析,分析结果显示,22种PAEs在该范围内的线性关系良好,相关系数均大于0.995,方法的平均回收率为82.9%～108.9%,相对标准偏差为0.9%～11.2%。同时,使用增强子离子扫描谱图进行搜库匹配,定性准确性高。该方法适用于饮用水中PAEs的检测。     

苦味酸测定中关键问题的研究

目前测定苦味酸的国标方法为《生活饮用水标准检验方法有机物指标》(GB/T 5750.8—2006)中的衍生物-液液萃取-气相色谱法,在实际测试过程中,发现水样pH值和基质效应会影响苦味酸测定。当pH值为8~12时,生成的氯化苦响应强度变化不大;在pH约为13时,响应强度最大。水质中除腐殖酸、硝基甲烷及2,4,6-三硝基甲苯会影响苦味酸测定外,硝基酚类和甲基酚类同样起到正干扰作用,因此,国标方法不能全面和准确地测定水中的苦味酸含量。     

Plant steroid hormones produced under Ni stress are involved in the regulation of metal uptake and oxidative stress in Brassica juncea L

Brassinosteroids (BRs) are involved in the amelioration of various biotic and abiotic stresses. With an aim to explore the role of BRs under heavy metal stress, plants of Brassica juncea L. were grown in pots. The plants were subjected to various concentrations of Nickel metal (0.0, 0.2, 0.4 and 0.6 mM) and harvested on 60th day in order to observe the expression of these hormones. The isolated BRs from the leaves of Brassica plants characterized by GC-MS include 24-Epibrassinolide (24-EBL), Castasterone, Dolicholide and Typhasterole. The effect of isolated 24-EBL was studied on Ni metal uptake and antioxidative defense system in 60 d old plants of Brassica. It was observed that 24-EBL significantly increased the activities of stress ameliorating enzymes and lowered the metal uptake in plants. This is the first report in B. juncea L. plants showing the expression of BRs under metal treatments and effect of the isolated 24-EBL on metal uptake and in oxidative stress management.