Comparative evaluation of Fe(III) reducing power-based antioxidant capacity assays in the presence of phenanthroline, batho-phenanthroline, tripyridyltriazine (FRAP), and ferricyanide reagents

The chemical diversity of antioxidants in complex matrices such as plant extracts makes it difficult to separate and quantify antioxidants from these solutions. Therefore it is desirable to establish methods that can measure the total antioxidant capacity (TAC) levels directly from plant extracts. Iron(III)-based TAC assays, especially the most widely used FRAP (ferric-reducing antioxidant power), play an important role in this regard. However, many problems have been reported in the application of the FRAP assay, the most serious one being the incomplete oxidation of a number of antioxidants during the time protocol of the assay. Thus, six different ferric ion-based total antioxidant capacity (TAC) assays have been comparatively tested, modified, and improved so as to obtain more sensitive and precise results for complex mixtures, namely: 1,10-phenanthroline (o-phen) method (with incubation), batho-phenanthroline method (with incubation), original FRAP method, modified FRAP method (with incubation), original ferricyanide method, and modified ferricyanide method (with incubation). Two new assays in this regard (i.e., o-phen and batho-phen) have been established, and the existing assays (FRAP and ferricyanide) have been modified so as to let the oxidation reactions of antioxidants reach completion. The molar absorptivity for a variety of antioxidants was highest for modified FRAP, batho-phen, and original FRAP methods. The absorption maximum wavelength shifted batochromically to a higher extent for modified ferricyanide, FRAP, and batho-phen procedures, decreasing the possibility of interferences due to organics absorbing in the near-UV range of the visible spectrum where most antioxidant assays are performed. The linear concentration ranges were shown to be further extended and linear correlation coefficients improved with respect to the most widely used ferric-based assay, FRAP. Of the six assays tested and developed, only the modified ferricyanide procedure gave high intercept values and low addivitity of TAC values of constituents in complex mixtures, requiring further attention of method optimization. Thus, it was shown that the most widely used FRAP could be effectively modified, and o-phen, batho-phen, and ferricyanide methods constitute cheaper alternatives to FRAP under certain conditions, with partly improved molar absorptivity (and thus sensitivity) for antioxidants, lower intercept values (and higher precision), broader linear range (and higher flexibility), and better additivity of TAC values of antioxidant constituents in mixtures.     

Kinetics of epidermal growth factor/receptor binding on cells measured by total internal reflection/fluorescence recovery after photobleaching

Total internal reflection fluorescence (TIRF) microscopy is used to measure the dissociation kinetic rate of fluorescein-labeled epidermal growth factor from its specific receptors on the surface of intact but mildly fixed A431 human epidermoid cells in culture. Prior applications of TIRF microscopy have been limited to nonreceptor binding or to model membrane systems. The evanescent field excites fluorescence selectively at the surface of the cell proximal to the coverslip. Prismless epiillumination TIR is employed to avoid space limitations and is achieved by passing the excitation laser beam through a high (1.4)-aperture objective so that the light is incident at the glass/water interface beyond the critical angle. Long-term focus is maintained by a special feedback system. Of the possible effects that can influence the time course of the postbleach fluorescence recoveries—the EGF/receptor dissociation ratek ₂, the bulk solution diffusion rate of EGF, and the cell surface motion of the receptors—we infer that the dissociation ratek ₂ dominates. Several fitting schemes are compared and indicate the presence of a multiplicity of values fork ₂, ranging from about 0.05 to 0.004 s^–1, with an average value of about 0.012 s^–1. These results compare well with values previously obtained by radiolabel/washing techniques. The significance of the results in terms of kinetic models and the advantages of the TIRF technique for these sorts of measurements are discussed.     

Element determination in medieval soil samples by total reflection X-ray fluorescence analysis

An aqua regia extraction procedure for heavy metals in soils optimised for total reflection X-ray fluorescence analysis is presented. The procedure is applied to 92 soil samples of medieval layers from the city area of Dortmund. Sixteen elements (P, S, K, Ca, Ti, Cr, Mn, Fe, Ni, Cu, Zn, Rb, Sr, Ag, Sn, and Pb) were used to characterise 17 sample sites. The results are projected onto the medieval urban structure of Dortmund. Two sites loaded with non-ferrous heavy metal could be detected and correlated with archaeological data. The efficiency and repeatability of the proposed extraction procedure is discussed.     

Analysis of low Z elements on Si wafer surfaces with synchrotron radiation induced total reflection X-ray fluorescence at SSRL, Beamline 3-3: comparison of droplets with spin coated wafers

The unique properties of synchrotron radiation, such as high incident flux combined with low divergence, its linear polarization and energy tunability, make it an ideal excitation source for total reflection X-ray fluorescence (TXRF) spectroscopy in order to non-destructively detect trace impurities of transition metals on Si wafer surfaces. When used with a detector suitable for the determination of low energy radiation this technique can be extended to the detection of low-Z elements, such as Al, Na and Mg. Experiments have been performed at SSRL Beamline 3-3, a bending magnet beamline using monochromatic radiation from a double multilayer monochromator. The wafer was mounted vertically in front of the detector, which was aligned along the linear polarization vector of the incoming synchrotron radiation. This configuration allows the detector to accept a large solid angle as well as to take advantage of the reduced scattered X-ray intensity emitted in the direction of the linear polarization vector. A comparison between droplet samples and spin coated samples was done, in order to compare the capabilities of vapor phase decomposition (VPD-TXRF) with conventional SR-straight-TXRF. Detection limits in the range of 50 fg corresponding to 2E10 atoms/cm² have been obtained for Na. The spin coated samples, prepared from solutions containing an equal amount of Na, Mg and Al showed an unexpected result when performing a scan of the angle of incidence of the incoming X-rays suggesting a different adsorption behavior of the elements in a multielement solution on the wafer surface. The observation of this behavior is important because the spin coating technique is the standard method for the preparation of surface standards in semiconductor quality control. This effect could be characteristic of the Na, Mg, Al solution used, but the angle dependence of the fluorescence signal of a standard should always be investigated before using the standard for calibration of the apparatus and quantification.     

Immunosensor for estrone with an equal limit of detection as common analytical methods

Immunoanalytical methods at a very low limit of detection (LOD) and a low limit of quantification (LOQ) are becoming more and more important for environmental analysis and especially for monitoring drinking water quality. Biosensors have suitable characteristics such as efficiency in allowing very fast, sensitive, and cost-effective detection. Here we describe a fully automated immunoassay for estrone with a LOD below 0.20 ng L^–1 and a LOQ below 1.40 ng L^–1. In contrast to common analytical methods such as GC-MS or HPLC-MS, the biosensor used requires no sample pre-treatment and pre-concentration. The basis of our sensitive assay is the antibody with a high affinity constant towards estrone. The very low amount of antibody per sample results in low validation parameters (LOD, LOQ, and IC50), but this assay for estrone represents the current device-related limitation of the River Analyser (RIANA).     

青藏铁路清水河段多年冻土区站场路基的试验研究

通过对青藏铁路清水河段站场路基的初步试验,获取了地温变形数据,探讨站场路基的冻结和融化过程的规律.实验表明:站场路基下冻土人为上限发生了上移,多年冻土得到了保护,为类似路段多年冻土工程提供借鉴.     

中国境内IGS站数据处理及地壳运动研究

利用中国境内国际GPS大地测量和地球动力学服务(IGS)站的GPS单天数据,使用GAMIT软件对其进行基线解算.以单天解的基线结果作为输入量,利用所介绍的台站漂移数学模型,求解台站漂移速度,得到地壳运动信息;再根据板块运动欧拉定理,求解中国大陆整体的欧拉矢量.结果表明,在ITRF2000框架下,求解的台站漂移速度与IGS公布的结果相近,由此求解的中国大陆整体的欧拉矢量与采用IGS公布数据计算的结果相近.     

水下作业工具深水液压动力源

研究了深水液压动力源的有关问题,探讨了水压力自动补偿器组成、原理及作用,介绍了自动补偿式深水液压动力源的工作原理、组成、压力自动补偿器的结构,论证并推导出水压力自动补偿器容积公式,研制了深水液压动力源,并进行了系统试验.     

泵站枢纽三维湍流数值模拟研究

采用雷诺平均纳维斯托克斯方程(RANS)和标准κ-ε湍流模型,运用SIMPLEC算法,对无锡市仙蠡桥泵站枢纽6种运行组合工况进行了三维数值模拟,预测了回流区及旋涡发生的位置和形态,计算得出了泵站枢纽流速分布规律以及泵站出水河道与京杭大运河交汇处的最大横向流速,计算结果与水工模型试验结果吻合.该研究不仅为仙蠡桥泵站枢纽优化设计、合理布局提供了理论指导,而且研究方法可应用于其他泵站枢纽水流流态数值模拟.     

微波协助萃取地锦草中总黄酮

采用微波辅照诱导萃取法萃取地锦草中的总黄酮，将试剂微量化后，通过对提取条件的研究得出较佳的工艺条件为：提取溶剂为70％的乙醇，固液比为(g／ml)1：10，微波功率为800W，辅照时间50s，提取次数为3次．