Coupled liquid chromatography-gas chromatography for the rapid analysis of gamma-oryzanol in rice lipids

An approach based on on-line coupled liquid chromatography-gas chromatography (LC-GC) was developed for the rapid analysis of gamma-oryzanol in rice. Total lipids were extracted from rice and subjected to LC-GC without any prior purification. gamma-Oryzanol was pre-separated by HPLC from rice lipids and transferred on-line to GC analysis in order to separate its major constituents. 24-methylenecycloartanyl ferulate, cycloartenyl ferulate, campesteryl ferulate, beta-sitosteryl ferulate and campestanyl ferulate. The identities of the compounds were confirmed by off-line GC-MS analysis. Total gamma-oryzanol content could be quantified by HPLC-UV detection and the distribution of gamma-oryzanol constituents could be determined by on-line coupled GC analysis. The proposed methodology paves the way for high-throughput investigations providing information on natural variations in gamma-oryzanol content and its composition in different rice varieties.     

Electrokinetic investigations of charged porous membranes

Asymmetric ultrafiltration membranes were prepared from fully aromatic polyamides differing in the diamine monomers of the polymeric backbone and from polysulfone. Nanofiltration membranes were made from polysulfone and polyethersulfone. The polysulfone as well as the polyethersulfone were chemically modified to change the surface charges of the membranes that were made from these polymers. This means neutral, positively as well as negatively charged membranes could be employed for the measurements. The surface properties of the membranes as a function of pH were determined by measuring the streaming potential in a perpendicular and horizontal mode. Applying proteins the values of the streaming potential changed depending on the original charges of the membranes as well as on the pH of the solution. The values shifted to either higher or lower absolute values. Thus, characterization of unused and used membranes can be carried out by electrokinetic measurements. This was also demonstrated using a membrane fitted out with invertase. The zeta potential of nanofiltration membranes, however, was only evaluated from the results obtained with the horizontally run cell.     

Composition and properties of freeze-dried products of nicotinic acid withβ-cyclodextrin and heptakis (2,6-0-dimethyl)-β-cyclodextrin

The purpose of the study was to examine the formation of inclusion compounds in the freeze-dried products obtained from aqueous solutions of nicotinic acid and -cyclodextrin (-CD), or heptakis (2,6-0-dimethyl)--cyclodextrin (DIMEB). The molar ratios used were 1:1 and 2:1. In addition two freezing temperatures (–40 and –196°C) and different secondary drying temperatures (+50 and +80°C) were used. Freeze-dried products with -CD obtained after low temperature freezing are of the same crystallographic structure as seen in a pure inclusion compound prepared by coprecipitation. Amorphous products were formed after fast freezing. The molar ratios of included nicotinic acid in the freeze-dried products vary — dependent on the preparation conditions — between 0.75:1 and 1:1. A factorial design proves that the included drug amount can be increased by enhancement of the amount of nicotinic acid used, by faster freezing, and by the combination of these two factors. The proof of inclusion formation was given by a combination of X-ray diffractography, differential scanning calorimetry, thermogravimetry and thermofractography.The freeze-dried preparations obtained with DIMEB were amorphous mixtures of the two components. No proof for inclusion of the nicotinic acid in the cyclodextrin cavity could be given. Higher (–40°C) or lower (–196°C) freezing temperatures and the running of the secondary drying process could not influence these results. The very low stability constant of the complex and steric reasons are responsible for this behavior.     

Über die bei hohen Ansäuerungsgraden auftretenden Polymolybdat-Typen,insbesondere zur Frage der „Dekamolybdate”︁ und „Phase C”︁-Polymolybdate

On the Polymolybdate Types Occurring at High Degrees of Acidification, with Particular Reference to the “Decamolybdates” and “Phase C” Polymolybdates It is shown that in the range of high acidification (> 1.6H⁺/MoO₄^2?) of aqueous molybdate solutions only two types of solid polymolybdates occur, namely the 36-molybdate and the “decamolybdate” types. These types can be most conveniently identified by their Raman spectra and also by some other characteristics. All the other polymolybdate types proposed in the literature for this range of acidification (“hexamolybdates”, “octamolybdates”, “dodecamolybdates”, “16-molybdates”, a 19-molybdate, the large group of polymolybdates characterized by a wide range of b in the general formula M₂O · bMoO₃ · cH₂O, “phase C” polymolybdates, a “hexagonal hydrate of molybdenum trioxide”, a “reactive molybdic acid”, “NH₃(MoO₃)₃”, and others) can be assigned to one of these two types. The most important reason for the erroneous assignments in the literature is the isomorphous exchange of varying quantities of the alkali or alkaline earth metal cations by H₃O⁺ in the crystal structure, occurring in the highly acidic solutions, particularly with the small cations. This cannot be recognized by the presently available methods of investigation and, hence, leads to the creation of new polymolybdate types. Another reason causing some of the confusion is the assignment of virtually identical X-ray diffraction data to two different types of lattices, a hexagonal and cubic lattice.     

Investigation,Modelling and Analysis of stiffened GFRP-Samples

Glasfibre structures feature high potentials for optimization and substitution of conventional materials like steel and aluminum and their alloys. The paper deals with the insertion of glasfibre trusses into thin glasfibre structures to reinforce them. The effective material properties of the glasfibre structures were estimated by experiments and simulations. Furthermore the Young's modulus of the trusses was obtained by bending tests and tension tests. A comparison between bending experiments and bending simulations is given. (© 2006 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim)     

Calculating the variance of errors in population forecasting

For judging the quality of population forecasting methods, the root mean square error (RMSE) has proven to be a useful tool. A suitable variance component model is proposed for calculating the variance of the RMSE. The method is demonstrated by an example.