Separation ofAstragalus saponins by reversed phase high performance liquid chromatography and evaporative light scattering detection

Summary A new HPLC method permitted the separation of 13 triterpene lycosides isolated from differentAstragalus species within 40 min. A water/acetonitrile gradient was used as eluent and 5 μm RP-18 material as stationary phase. By using an evaporative light scattering (ELS) detector, the main saponins ofA. membranaceus could be detected at levels as low as 20.0 μg·mL⁻¹. This method facilitated distinction of differentAstragalus species as well as the analyses of market products containingA. membranaceus. The results showed variations from 0.019 to 0.184% in the total saponin content of the market products.     

Separation ofCimicifuga racemosa triterpene glycosides by reversed phase high performance liquid chromatography and evaporative light scattering detection

Summary The main triterpene glycosides ofCimicifuga racemosa were separated by reversed phase HPLC, using a C-18 column, Evaporative Light Scattering (ELS) detection and a grient system consisting of water, acetonitrile and reagent alcohol. Within 35 min three main glycosides could be separated and quantified in the methanolic root extract with detection limits of 10.5, 15.6 and 31.6 μg·mL⁻¹ respectively. The method was successfully used, to analyzed differentCimicifuga racemosa market products, as well as to distinguish between otherCimicifuga samples from China.     

Mechanism of Butane Transformation

Catalytic activity and aromatic selectivity of n‐butane transformation were studied over various MFI type zeolites. From the data obtained, a reaction mechanism is suggested for different catalyst systems. It is visualized that in gallium doped catalysts, Ga³⁺ directly takes part both in cracking and dehydrogenation. The [Ga CH₃]²⁺ and [GaH]²⁺ species formed during cracking and dehydrogenation require protonic sites for regeneration of Ga³⁺ species. An alternative mechanism was suggested for dehydrogenation and cracking by Ga³⁺ without the involvement of protonic sites. However a protonic site would be required for aromatization. In case of gallosilicates a one step mechanism is suggested for cracking and dehydrogenation reaction which does not require the presence of protonic sites in the catalyst system.     

A Characterisation of a Class of Semigroups with Locally Commuting Idempotents

McAlister proved that a necessary and sufficient condition for a regular semigroup S to be locally inverse is that it can be embedded as a quasi-ideal in a semigroup T which satisfies the following two conditions: (1) T = TeT, for some idempotent e; and (2) eTe is inverse. We generalise this result to the class of semigroups with local units in which all local submonoids have commuting idempotents.     

Evolution of subsequent yield surfaces and elastic constants with finite plastic deformation. Part-I: A very low work hardening aluminum alloy (Al6061-T6511)

In the present study, the initial and subsequent yield surfaces in Al 6061-T6511, based on 10 με deviation from linearity definition of yield, are presented. The subsequent yield surfaces are determined during tension, free end torsion, and combined tension–torsion proportional loading paths after reaching different levels of strains. The yield surfaces are also obtained after linear, bi-linear and non-linear unloading paths after finite plastic deformation. The initial yield surface is very close to the von-Mises yield surface and the subsequent yield surfaces undergo translation and distortion. In the case of this low work hardening material, the size of the yield surfaces is smaller and negative cross-effect is observed with finite plastic deformation. The subsequent yield have a usual “nose” in the loading direction and flattened shape in the reverse loading direction; the observed nose is more dominant in the case of tension and combined tension–torsion loading than in torsional loading. The size of the yield surfaces after unloading is smaller than the initial yield surface but larger than subsequent yield surfaces obtained during prior loading, show much smaller cross-effect, and the shape of these yield surfaces depends strongly on the loading and unloading paths. Elastic constants (Young’s and shear moduli) are also measured within each subsequent yield surfaces. Evolution of these constants with finite deformation is also presented. The decrease of the two moduli is found to be much smaller than reported earlier in tension by Cleveland and Ghosh [Cleveland, R.M., Ghosh, A.K., 2002. Inelastic effects on springback in metals. Int. J. Plast. 18, 769–785]. Part-II and III [(Khan et al., 2009a) and (Khan et al., 2009b)] of the papers will include experimental results on annealed 1100 Al (a very high work hardening material) and on both Al alloys (Al6061-T6511 and annealed 1100 Al) in tension- tension stress space, respectively. The results for both cases are quite different than the ones that are presented in this paper.     

Crystal structure of cholest-4-ene-3,6-dione: A steroid

The crystal structure of cholest-4-ene-3,6-dione (C₂₇H₄₄O₂) has been determined by X-ray diffraction methods. The compound crystallizes in the monoclinic crystal system (space group P2₁) with the unit cell parameters a = 10.503(4) Å, b = 8.059(1) Å, c = 14.649(1) Å, β = 105.4(2)°, and Z = 2. The structure has been refined to an R value of 0.035 for 2252 observed reflections. Ring A of the steroid nucleus exists in a sofa conformation, while rings B and C adopt a chair conformation. The five-membered ring D exhibits a half-chair conformation. The molecules in the unit cell are linked together by the C-H?O hydrogen bonds.     

Rheology and gelation of cellulose/ammonia/ammonium thiocyanate solutions

Liquid crystalline solutions of cellulose in an ammonia/ammonium thiocyanate solvent will form thermoreversible gels at temperatures below 30°C. These gels are of interest both for processing the cellulose/ammonia/ammonium thiocyanate system and because they have an unusual structure, containing neither crystalline nor covalently bonded crosslinks. Although these gels contain neither crystalline nor covalently bonded crosslinks, the dynamic rheological behavior of the system at the gel point was found to be the same as for gels with covalent or crystalline crosslinks with a loss tangent, tan δ, independent of frequency. The kinetics of the gelation process was monitored via dynamic elastic modulus, G′. All samples revealed an exponential increase in G′ with time during gelation, very different from that observed in covalently bonded or crystalline crosslinked systems. Measurements of the loss tangent enabled precise determination of the gelation time for these systems as a function of cellulose concentration and temperature. We found the gel time to be inversely related to cellulose concentration and directly related to temperature. The strong dependence of gel time on these parameters offers a windows of spinnability that can be tailored for processing high modulus cellulose fibers. © 1996 John Wiley & Sons, Inc.     

Chromophore and spectrum of the glycogen–iodine complex

The experimental UV-vis spectrum of the glycogen-iodine (GI) complex shows certain features remarkably similar to that of the amylopectin-iodine (API) complex [J. Polymer. Chem. 32, 2257 (1994)], suggesting a strong similarity between the API and the GI structures. As in the API complex, a nearly linear polyiodine unit, I₄, at an interiodine distance of around 3 Å is expected to exist within the helix of 11 anhydroglucose units (AGUs). There are several other spectral features that suggest the presence of another similar but more loosely bound iodine species with a longer interiodine distance of 3.1 Å. These findings suggest the involvement of two different types of glycogen chains in binding iodine molecules. © 1996 John Wiley & Sons, Inc.     

Kinetic studies on general base-catalyzed cleavage of phthalimide (PTH) in 2-hydroxyethylamine and 2-methoxyethylamine buffers

Kinetic studies on the nucleophilic cleavage of phthalimide (PTH) in buffers of 2-hydroxyethylamine and 2-methoxyethylamine reveal nonlinear plots of k_n vs. [Buf]_T (at constant pH) where k_n and [Buf]_T represent apparent second-order rate constant and total amine buffer concentration, respectively. The nonlinear variation of k_n against [Buf]_T is attributed to the occurrence of a stepwise mechanism in the aminolysis of PTH. Intermolecular general base catalysis is detected in the reactions of both amines with nonionized PTH (SH) only within the pH range of the present study. © 1996 John Wiley & Sons, Inc.     

Phase Transition Energy of the Short Period Basic Polytypes of CdI2

The CdI₂ material grown under similar thermodynamic conditions exhibits several polytypes (phases). Out of these the basic phases are thermodynamically independent and grow with their minimum free (potential) energy. In the present paper we have calculated the Madelung constants cohesive (potential) and the phase transformation energy for the basic phases viz. 2H → 4 H.