Chemische Vitamin D<Subscript>3</Subscript>-Bestimmung in Lebertran

The different aspects of Vitamin D₃ determination and the data reported in the literature are discussed. The spectrophotometric determination of Vitamin D₃ in cod-liver oil is carried out after the alkaline saponification, extraction of unsaponified parts, precipitation of accompanying sterols and the column- and thin-layer chromatographic purification and separation of vitamin D₃ on 40 cm plates from other vitamins. The dyestuff α-naphtholbenzein is suited well as standard substance for the better location and identification of vitamin D₃ zone on the thin-layer plate. The results obtained from the chemical method were checked through the simultaneous biological determination.     

Characterization of oligosaccharide moieties of intact glycoproteins by microwave-assisted partial acid hydrolysis and mass spectrometry

A method, which utilizes microwave-assisted partial acid hydrolysis and matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOFMS), to elucidate oligosaccharide composition of intact glycoproteins is presented here. Glycoproteins, such as ribonuclease B, avidin, alpha1-acid glycoprotein, and fetuin, are used as model systems to demonstrate this technique. Partial cleavage of oligosaccharides from whole intact glycoproteins with trifluoroacetic acid was observed after a short exposure to microwaves. Due to the high-resolution mass spectra obtained by MALDI-TOFMS from glycoproteins with molecular weights less than 20 kDa, the compositions of oligosaccharides are readily derived for ribonuclease B and avidin. The data agree with the proposed oligosaccharide structures of ribonuclease B (five glycoforms) and avidin (eight glycoforms). Larger glycoproteins such as alpha1-acid glycoprotein (many glycoforms) and fetuin (many glycoforms) exhibited only broad peaks with no glycoform resolution. Nevertheless, this method can be used successfully for analysis of glycoproteins with molecular weights greater than 20 kDa to determine the presence or absence of glycosylation.     

Studies of tetracene- and pentacene-based organic thin-film transistors fabricated by the neutral cluster beam deposition method

The neutral cluster beam deposition (NCBD) method has been applied to produce and characterize organic thin-film transistors (OTFTs) based upon tetracene and pentacene molecules as active layers. Organic thin films were prepared by the NCBD method on hexamethyldisilazane (HMDS)-untreated and -pretreated silicon dioxide (SiO2) substrates at room temperature. The surface morphology and structures for the tetracene and pentacene thin films were examined by atomic force microscopy (AFM) and X-ray diffraction (XRD). The measurements demonstrate that the weakly bound and highly directional neutral cluster beams are efficient in producing high-quality single-crystalline thin films with uniform, smooth surfaces and that SiO2 surface treatment with HMDS enhances the crystallinity of the pentacene thin-film phase. Tetracene- and pentacene-based OTFTs with the top-contact structure showed typical source-drain current modulation behavior with different gate voltages. Device parameters such as hole carrier mobility, current on/off ratio, threshold voltage, and subthreshold slope have been derived from the current-voltage characteristics together with the effects of surface treatment with HMDS. In particular, the high field-effect room-temperature mobilities for the HMDS-untreated OTFTs are found to be comparable to the most widely reported values for the respective untreated tetracene and pentacene thin-film transistors. The device performance strongly correlates with the surface morphology, and the structural properties of the organic thin films are discussed.     

Composition-controlled synthesis of bimetallic gold-silver nanoparticles

This paper reports findings of an investigation of the synthesis of monolayer-capped binary gold-silver (AuAg) bimetallic nanoparticles that is aimed at understanding the control factors governing the formation of the bimetallic compositions. The synthesis of alkanethiolate-capped AuAg nanoparticles was carried out using two related synthetic protocols using aqueous sodium borohydride as a reducing agent. One involves a two-phase reduction of AuCl(4)(-), which is dissolved in organic solution, and Ag(+), which is dissolved in aqueous solution. The other protocol involves a two-phase reduction of AuCl(4)(-) and AgBr(2)(-), both of which are dissolved in the same organic solution. AuAg nanoparticles of 2-3 nm core sizes with different compositions in the range of 0-100% Au have been synthesized. The two synthetic routes were compared in terms of bimetallic composition and size properties. Our new findings have allowed us to establish the correlation between synthetic feeding of metals and metal compositions in the bimetallic nanoparticles, which have important implications to the exploration of gold-based bimetallic nanoparticles for constructing sensing and catalytic nanomaterials.     

Estimation of Multinomial Probabilities under a Model Constraint

In this paper estimation of the probabilities of a multinomial distribution has been studied. The five estimators considered are: unrestricted estimator (UE), restricted estimator (RE) (under model ), preliminary test estimator (PTE) based on a test of the model , shrinkage estimator (SE) and the positive-rule shrinkage estimator (PRSE). Asymptotic distributions of these estimators are given under Pitman alternatives and the asymptotic risk under a quadratic loss has been evaluated. The relative performance of the five estimators is then studied with respect to their asymptotic distributional risks (ADR). It is seen that neither of the preliminary test and shrinkage estimators dominates the other, though each fares well relative to the other estimators. However, the positive rule estimator is recommended for use for dimension 3 or more while the PTE is recommended for dimension less than 3.     

Evaluation of the quality of colour changes of complexometric indicators in the titration of copper (II) with EDTA by tristimulus colorimetry

The quality of colour changes of the indicators hematoxylin, 4(2-pyridylazo)resorcinol (PAR), xylenol orange, pyrocatechol violet, chromazurolS and eriochrome cyanineR in the complexometric titration of copper(II) with ethylenediaminetetraacetic acid (EDTA) were studied with the help of tristimulus colorimetry, utilising a comparative study of the parameters SCD (specific colour discrimination), CIE La^*b^* 1976 and LABHNU 1977. Hematoxylin was found to be the best indicator among those studied. A screened indicator, viz. PAR + malachite green (52), was developed to enhance the quality of colour transition at the end-point and the accuracy of the titrimetric determination.     

Chelating ion-exchangers containing n-substituted hydroxylamine functional groups: Part 6. Sorption and separation of gold and silver by a polyhydroxamic acid

The sorption and desorption characteristics of gold and silver on a polyhydroxamic acid chelating resin are described. Gold is quantitatively sorbed from 0.5 M nitric acid or neutral solutions, and readily eluted with 0.5% ($\text{w}\text{v}$) potassium cyanide solution. Silver is removed from 0.05 M nitric acid or neutral solutions, and can be eluted with the cyanide solution or with 0.5 M nitric acid. Gold can be quantitatively separated from copper, iron and silver; gold and silver are sorbed from dilute cyanide solutions. Tests with river water and other eluting systems are reported.     

Complexation of Fluvastatin Sodium with β-Cyclodextrin: NMR Spectroscopic Study in Solution

¹H NMR spectroscopic study of fluvastatin sodium (FLU), β-Cyclodextrin (β-CD) and their mixtures confirmed the formation of FLU/β-CD inclusion complex in solution. The stoichiometry of the complex was determined to be 1:1 and the overall binding constant (K _s) was calculated to be 340 M⁻¹. Two dimensional COSY, ROESY and DEPTO experiments were performed for the unambiguous assignment of aromatic proton resonances and it was found that two isomeric forms of FLU are present in solution. It was confirmed with the help of ROESY spectral data that only F-substituted aromatic ring penetrates the β-CD cavity and there is chiral differentiation by the β-CD as one of the isomer binds more strongly, which is indicated by the intensity of correlation peaks. The mode of penetration of the guest into the β-CD cavity was also established and structure of the complex has been proposed.     

Spectroscopic Study on Interaction of β-Cyclodextrin with Triprolidine Hydrochloride

The complexation of triprolidine hydrochloride （TRP） and β-cyclodextrin （β-CD） in deuterium oxide was investigated by 400 MHz 1^H NMR spectroscopy. The 800 MHz 2D ROESY data revealed that two 1 ：1 and one 2 ： 1 β-CD-TRP inclusion complexes were formed. Both aromatic moieties （p-tolyl and pyridyl ring） has entered into the β-CD cavity, confirming the existence of two different equilibria for 1 ： 1 inclusion complexes in which p-tolyl ring of the guest is more tightly held by the host cavity. The ROE intermolecular interactions provided the plausible structures of these 1 ： 1 and 2 ： 1 stoichiometric inclusion complexes of β-CD-triprolidine hydrochloride in solu- tion.     

Unexpected, drastic effect of triflic acid on oxidative diacetoxylation of iodoarenes by sodium perborate. A facile and efficient one-pot synthesis of (diacetoxyiodo)arenes

An easy, safe, and effective method for preparing (diacetoxyiodo)arenes from iodoarenes is presented. Addition of trifluoromethanesulfonic acid (triflic acid) as a promoter causes a drastic increase in the yield of (diacetoxyiodo)arenes in the reaction of iodoarenes with sodium perborate. The reaction of the iodoarenes with sodium perborate in acetic acid in the presence of triflic acid at 40-45 degrees C efficiently generates the corresponding (diacetoxyiodo)arenes in high yields within short time.