五种中药中微量元素及重金属元素的含量分析

用微波消解-原子吸收分光光度法对巴戟天、大黄、陈皮、板蓝根、茯苓等5种中药材中的7种金属微量元素进行了含量分析。结果表明,该法的线性良好,重现性在3.3%~11%之间,精密度在2.6%以内,回收率满足定量分析要求;5种药材中铅均未超标,茯苓中镉超出国家标准;5种药材里的铜含量均有超标,其中,巴戟天超标最严重;铁在5种药材中的含量最高,其中以巴戟天含量最为丰富,达到了746.750 mg/kg,其次是锌和锰,铬的含量最少。结论:对5种药材中铜均出现超标,虽然在边缘位置,但应该予以重视;巴戟天中丰富的铁元素,可能在防止癌变发生和发展中起到一定功效。     

中国微量元素科学研究现状、意义、问题和对策

通过"从统计数字看现状"、"从科研成果看意义"、"从社会现象看问题"和"为持续发展想对策"等四个方面高度概括了中国微量元素科学研究走过的30多年历程,为该学科今后的持续发展提供了方向性的意见和讨论的基础。     

Problems,possibilities and limitations of inductively coupled plasma atomic emission spectrometry in the determination of platinum,palladium and rhodium in samples with different matrix composition

The economic and geological importance of platinum group of elements has led to the development of analytical methods to quantify them in different types of samples. In the present paper the quantitative information for spectral interference in radial viewing 40.68 MHz inductively coupled plasma atomic emission spectrometry in the determination of Pt, Pd and Rh in the presence of complex matrix, containing Al, Ca, Fe, Mg, Mn, P and Ti as matrix constituents was obtained. The database was used for optimum line selections. By using the selected analysis lines the following detection limits in ng g^− 1 were obtained: Pt 1700, Pd-1440, Rh-900. The reached detection limits determine the possibilities and limitation of the direct ICP-AES method in the determination of Pt, Pd and Rh in geological and environmental materials. The database for spectral interferences in the presence of aluminum can be used for the determination of platinum group of elements in car catalysts.     

Sample cleanup-free determination of mycophenolic acid and its glucuronide in serum and plasma using the novel technology of ultra-performance liquid chromatography-electrospray ionization tandem mass spectrometry

Mycophenolic acid (MPA) is an immunosuppressant drug which powerfully inhibits lymphocyte proliferation. Since the early 1990s it has been used to prevent rejection in organ transplantation. The requirement of therapeutic drug monitoring shown in previous studies raises the necessity of acquiring accurate and sensitive methods to measure MPA and its major metabolite mycophenolic acid glucuronide (MPAG).The authors developed a sample cleanup-free, rapid, and highly specific method for simultaneous measurement of MPA and MPAG in human plasma and serum using the novel technology of ultra-performance liquid chromatography-electrospray ionization tandem mass spectrometry. MPA- and MPAG-determinations were performed during a 2.0-min run time. Multiple calibration curves for the analysis of MPA and MPAG exhibited consistent linearity and reproducibility in the range of 0.05-100 (r > 0.999) mg L⁻¹ and 4-4000 mg L⁻¹ (r > 0.999), respectively. Limits of Detection were 0.014 mg L⁻¹ for MPA and 1.85 mg L⁻¹ for MPAG. Lower Limits of Quantification were 0.05 mg L⁻¹ for MPA and 2.30 mg L⁻¹ for MPAG. Interassay imprecision was <10% for both substances. Mean recovery was 103.6% (range 78.1-129.7%) for MPA and 111.1% (range 73.0-139.6%) for MPAG. Agreement was good for MPA and MPAG between the presented method and a validated HPLC-MS/MS method. The Passing-Bablok regression line for MPA and MPAG was HPLC-MS/MS = 1.14 UPLC-MS/MS—0.14 [mg L⁻¹], r = 0.96, and HPLC-MS/MS = 0.77 UPLC-MS/MS + 0.50 [mg L⁻¹], r = 0.97, respectively. This sample cleanup-free and robust LC-MS/MS assay facilitates the rapid, accurate and simultaneous determination of MPA and MPAG in human body fluids.     

Combination of several mass spectrometry ionization modes: a multiblock analysis for a rapid characterization of the red wine polyphenolic composition

In the present study, direct flow injection mass spectrometry was investigated for rapid characterization of the polyphenolic composition of red wines. Atmospheric pressure chemical ionization (APCI) and electrospray ionization (ESI) (in both positive and negative ion modes) have been simultaneously used for a more comprehensive analysis of the samples studied. In this way, four mass spectra have been recorded for each wine. Each spectrum was considered as a fingerprint related to the chemical composition. This methodology was applied to a large number of Beaujolais wines from different grades and different vintages.This data set was processed using a chemometrical multiblock analysis, which allowed to synthesize the whole information collected. The results obtained showed that the wine fingerprints address the composition of the main polyphenolic compounds present in the red wines and can discriminate groups of wines showing different polyphenolic compositions. Multiblock analysis appears as a very promising tool to deal with several data tables of multivariate signals in order to define, by combining the whole information, the best operating protocol according to the desired analytical objectives.     

Critical parameters in a supported liquid membrane extraction technique for ionizable organic compounds with a stagnant acceptor phase

The reviews cover important critical parameters that are often optimized in a supported liquid membrane extraction technique in both flat sheet and hollow fibre designs for ionizable organic molecules. Understanding of these parameters can enable one to predict the behavior of the compound before hand and thus reduce the number of optimization experiments. Moreover, less number of experiments can be also generated using statistical techniques which are now becoming more commonly used. Supported liquid membrane extraction optimal parameters such as the conditions of the pH of the acceptor and donor phases should easily be fixed from the pKa values of the compounds. Other parameters, including the polarity of the compound can help to predict the partitioning into the membrane and the behavior of the compound. The influence of parameters such as temperature on the mass transfer in supported liquid membrane depends on the design of the module, experimental design and type of mass transfer controlling the extraction process.     

多类型复发间隔时间下广义半参数风险模型

本文在多类型复发间隔时间数据下,研究了一类广义半参数风险回归模型的参数估计问题,给出了该模型中未知参数和非参数函数的一种估计方法,并证明了估计量的相合性和渐近正态性.最后利用数值模拟来评估估计量在有限样本下的表现.     

Modelling diffraction patterns from one‐dimensionally disordered structures of AIIBVI crystals by Monte Carlo Technique IV. The 6H structure with different kinds of stacking faults

To investigate the one‐dimensionally disordered structures (ODDS) in the close packed (cp) crystals, the Monte Carlo computer simulation technique has been applied. Calculations of the diffraction intensity distributions along the 10.L reciprocal lattice row from the 6H(33) structure with the four different kinds of the stacking faults (SFs): growth, deformation, layer displacement and extrinsic fault are presented. In particular, using the simple frequency functions of the fault to fault distances, both random and non‐random distributions of the SFs are considered. Distinctive features of the diffraction patterns corresponding to the chosen examples of the transformations from the parent 6H(33) structure into another small‐period polytypes are discussed in detail. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

标准镜的高精度柔性支撑镜框的优化设计

为了实现干涉仪标准镜中光学元件的高精度定位,设计了一种柔性支撑镜框,研究了该结构的力学模型、结构参数、定位精度和透镜变形。首先,根据材料力学原理将柔性镜框等效为一个弹簧系统;根据力学方程和几何关系,建立了透镜中心位置与柔性结构的挠度之间的二元方程。然后,分析了安装位置、温度、结构参数对透镜位置以及作用力的影响。最后,应用有限元仿真分析了所设计结构的力学性能,并进行对比验证。结果表明,数值仿真分析的结果与有限元仿真结果基本相同,柔性镜框的柔性结构厚度最优值为1.5 mm。该设计方案完全满足干涉仪标准镜对镜框在定位精度、稳定性方面的要求。     

二氧化碳探测仪典型透镜支撑结构的设计及分析(英文)

为了降低外界载荷和温度变化对二氧化碳探测仪光学系统透镜面形及共轴的影响,根据系统的特点和技术要求,对其典型透镜的支撑结构进行了研究,设计了一种径向挠性支撑结构并建立了3D实体模型。运用工程CAD分析软件,采用非线性有限元分析方法对其进行了动静刚度特性和热特性仿真分析,验证了支撑结构设计的合理性。分析结果表明,透镜结构组件的一阶固有频率为1 301 Hz;利用面型拟合,得到了各工况下镜面面形误差值为PV≤λ/10,RMS≤λ/50,偏转误差≤1″。该径向支撑结构能很好地保持透镜共轴精度,减小了温度变化对镜面变形的影响,各项结果满足设计要求,证明了结构设计的合理性。