Polarographic behaviour and determination of spironolactone

The polarographic behaviour of spironolactone in Britton-Robinson buffers containing 40% methanol as a solubilizer was studied. Over the pH range 3-12 a cathodic wave was produced. The wave was characterized as irreversible, diffusion-controlled and partially affected by adsorption phenomena. The number of electrons involved in the reduction was found by coulometric measurements at a controlled potential. A method was developed for the determination of spironolactone in tablets and the results obtained were in agreement with those obtained by the B.P. 1988 method. The mechanism of the electrode reaction is discussed.AvH scholar: 1989–1991     

Some observations on the automation by flow injection analysis of the spectrophotometric determination of amino acids and proteins witho-phthalaldehyde

Automation by flow injection analysis with Spectrophotometric detection of the determination of total amino acids and proteins witho-phthalaldehyde is not straightforward. The use of spectrophotometry, instead of spectrofluorimetry, and of N-acetyl-L-cysteine, instead of the conventional mercaptoethanol is advantageous because of the lower variability of absorptivities with respect to fluorescence yields, and the larger stability of the derivatives. Under adequate working conditions and with leucine as reference, the procedure can be used for the evaluation of total amino acids. A similar procedure is proposed for the analysis of proteins in a sample. Limits of detection are 1 × 10^–5 M for amino acids, and 1 × 10^–6 M for proteins, respectively.     

Electrochemical characterization of solid materials in volume range I. Chemical effects on the matrix-phase separation

The electrochemical phase isolation (EPI) is described as a preparation method for determining specific precipitations in solid materials in microamounts and microdimensions. Fundamental criteria are examined as a function of the main parameter (polarization current) on the system Fe₃C in a Fe-matrix. The influence of the electrolyte composition on the electrochemical behaviour of the matrix, on the one hand, and of the phase, on the other hand, are investigated and utilized.     

两种计算吸光光度法同时测定钙镁

研究了在pH10．5的硼砂-氢氧化钾缓冲溶液和乙醇的增敏作用条件下，偶氮氯膦Ⅰ与钙、镁的吸收特性，建立了多波长光度法同时测定钙和镁的方法。采用两种矩阵算法对试验数据进行处理，并对结果进行比较和分析。钙和镁含量在0～25μg／25ml范围内用计算法Ⅱ能得到准确结果。     

人中白矿物元素含量分析

用原子吸收分光光度法测定了中药人中白中 1 2种矿物元素含量。结果表明 ,人中白中Ca、Mg、Ba、K和Na的含量在 1× 1 0 3以上 ,而Fe、Cr、Mn的含量在 1 0× 1 0 6 ～ 1 0 0 0× 1 0 6 范围内 ;Ni、Se浓度也超过 1 0× 1 0 6 ,Cu、Co的含量也在 5× 1 0 6 以上。     

青海柴达木地区植物白刺叶中微量元素特征

青海柴达木地区分布有丰富的白刺植物资源。利用220FS原子吸收光谱仪分析了该地区三种白刺叶片的Cu,Zn,Fe,Mn,Cr,Ni,Cd等微量元素。结果表明，铬、 锰含量显著提高是青海柴达木地区植物白刺叶资源微量元素特征。这为柴达木地区白刺叶资源的开发利用提供科学依据。     

人参中总皂甙的超声波快速提取方法研究

建立了人参中总皂甙超声波半微量快速提取方法，与索氏提取法相比，此法提取时间由索氏法的1－2个工作日缩短到30min，节省大量试剂，综合提取效率提高数十倍，与索氏提取法对照分析表明，此法可完全满足人参中总皂甙的快速测定要求。     

Determination of Utratrace Silver Using Surfactant As Sensitizer by Catalytic Near Field Laser Thermal Lens Spectrometry

Thermal lens spectrometry (TLS) is an excellent tool for trace analysis1. TLS allows the detection of absorbances of 10-7～10-8, concentration of ≈ 10-11 mol稬-1 and the analysis of 10-15 L volumes with ≈10-2 absorbing molecules2. Kinetic analysis is playing an increasingly important part in modern analytical chemistry. Therefore, TLS shows much promise in combination with kinetic analysis. However, there are few data on TLS applications in kinetic analysis method so far3～4. A ne…     

Conformation and internal mobility of 5H-dibenzo[a,d]cycloheptene derivatives in solution. Conformational analysis of highly flexible structures,part II

Summary The conformational possibilities of 5-(3-N,N-dimethylaminopropyl)-5H-dibenzo[a,d]cycloheptene (1), 5-(3-N,N-dimethylaminopropylidene)-10,11-dihydro-5H-dibenzo[a,d]cycloheptene (2), and 5-(3-N,N-dimethylaminopropyl)-10,11-dihydro-5H-dibenzo[a,d]cycloheptene (3) are analysed using empirical force field methods. Minimum energy conformations, interconversion pathways, interconversion graphs and interconversion energies are examined in view of the analysis of conformer equilibria of1,2, or3 in solution. In addition, some basic requirements of the analysis of fast interconverting conformers using the lanthanide induced shift method are discussed.

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Konformation und interne Beweglichkeit von 5H-Dibenzo[a,d]cyclohepten Derivaten in Lösung. Konformationsanalyse hochflexibler Strukturen, Teil 2

Zusammenfassung Die konformativen Möglichkeiten von 5-(3-N,N-dimethylaminopropyl)-5H-dibenzo[a,d]cyclohepten (1), 5-(3-N,N-dimethylaminopropylidene)-10,11-dihydro-5H-dibenzo[a,d]cyclohepten (2) und 5-(3-N,N-dimethylaminopropyl)-10,11-dihydro-5H-dibenzo[a,d]cyclohepten (3) wurden mit Hilfe empirischer Kraftfeldmethoden analysiert. Jene Konformationen, die einem energetischen Minimum entsprechen, sowie Interkonversionswege, Interkonversionsgraphen und Interkonversionsenergien wurden in Hinblick auf die Analyse der Konformerengleichgewichte von1,2 oder3 in Lösung untersucht. Weiters werden noch einige grundlegende Voraussetzungen für die Analyse von sich schnell ineinander umwandelnden Konformeren mittels der Lanthaniden-induzierten Verschiebungsmethode besprochen.

     

胶束介质在动力学分析中的应用

评述了胶束介质在动力学分析测定中的作用和应用状况，讨论了胶束催化的动力学特征，胶束对反应物理化学性质的修饰及其在动力学多组份测定和酶催化动力学分析中的应用。