Simple high-performance liquid chromatography method for alpha-tocopherol measurement in Rosmarinus officinalis leaves. New data on alpha-tocopherol content.

A simple HPLC method for vitamin E (alpha-tocopherol) measurement in the leaves of Rosmarinus officinalis has been developed and validated. It has enabled new data for alpha-tocopherol content to be established. The leaves, recently harvested, were dried in a microwave oven and crushed; then, alpha-tocopherol was directly extracted from portions of ground material with acetone, by probe sonication. After centrifugation the acetonic extract was analysed by HPLC with ergocalciferol (vitamin D2) added as internal standard and a gradient elution with a Nucleosil C18 column at 35 degrees C. Validation parameters of the method can be considered adequate. For standards: linearity is r=0.999, recovery is 100+/-2%, intra-assay precision has RSD=+/-3% and inter-assay precision has RSD=+/-6%. For samples: linearity is r=0.99, recovery: 93+/-7%, intra-assay precision has RSD=+/-4% and inter-assay precision has RSD=+/-7%.     

Fast liquid chromatography/multiple‐stage mass spectrometry of coccidiostats

Drugs that are used as medicines and also as growth promoters in veterinary care are considered as emerging environmental contaminants and in recent years concern about their potential risk to ecosystems and human health has risen. In this paper we used a method based on liquid chromatography/electrospray tandem mass spectrometry to analyze eight coccidiostatic compounds: diclazuril, dinitrocarbanilide (the main metabolite of nicarbazin), robenidine, lasalocid, monensin, salinomycin, maduramicin and nasarin. Multiple‐stage mass spectrometry (MSⁿ) based on the precursor ions [M+Na]⁺ (polyether ionophores), [M+H]⁺ (robenidine) and [M–H]^? (diclazuril and dinitrocarbanilide) was used to study the fragmentation of these compounds. MSⁿ data and genealogical relationships were used to propose a tentative assignment of the different fragment ions. Loss of water, decarboxylations, ketone β‐cleavages and rearrangement of cyclic ethers and amide groups were some of the fragmentations observed for these compounds. Liquid chromatography with a sub‐2 µm particle size column was coupled to tandem mass spectrometry (LC/MS/MS) allowing the separation of these compounds in less than 7 min. Method detection limits ranging from 11 to 71 ng L^?1 and run‐to‐run values in terms of relative standard deviation (RSD) (up to 12%) were obtained. Copyright © 2009 John Wiley & Sons, Ltd.     

Local forms of molecular mobility in copolymethacrylates containing side‐chain nonlinear optical chromophores

Local forms of molecular mobility of comb‐like random copolymethacrylates, containing side‐chain nonlinear optical chromophores and amyl‐ or octafluoroamyl‐groups, are studied. In the glassy state, two relaxation processes are found, which are due to reorientation of terminal polar groups (γ₂‐process) and rotation of chromophore groups about their long axes (β‐process). For octafluoroamyl‐containing copolymers, the γ₂‐process is superposition of the two molecular motions due to reorientation of terminal chromophore groups and ? CF₂H groups. The intensity and relaxation times in the range of the γ₂‐process depend on the chemical structure and concentration of chromophores in a copolymer. For the β‐process, the molecular mobility weakly depends on the chromophore structure, being mainly determined by the relative lengths of the rigid chromophore and flexible side chains. On the global spectrum of depolarization current it was observed the γ₁‐process due to reorientation of (CH₂)_n spacers between chromophore groups and copolymer backbone. © 2008 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 46: 1488–1496, 2008     

Acceptor levels in indium selenide. An investigation by means of the Hall effect,deep-level-transient spectroscopy and photoluminescence

Acceptor levels related to I, II, IV, and V group impurities in indium selenide are studied by means of the Hall effect, deep-level-transient spectroscopy (DLTS) and photoluminescence. Activation energies for hole concentrations in the range from 200 to 300 meV have been measured. A reversible change of sign of the Hall voltage has been observed below 215 K. This behaviour can be explained through a model in which acceptor levels are assumed to be shallow and interlayer planar precipitates of ionized shallow donors create potential wells that behave as deep donors and in which a low concentration of bidimensional free electrons can exist. This model also explains the capacitance-voltage characteristics of both ITO/p-InSe and Au/p-InSe barriers. DLTS results are coherent with this model: hole traps in high concentration located about 570 meV above the valence band are detected. Photoluminescence also confirms the shallow character of acceptor levels. A broad band whose intensity is related to p conductivity appears in the PL spectra of low resistivity p-InSe. The shape and temperature dependence of this band can be explained through self-activated photoluminescence in a complex center in which the ground acceptor level must be at about 50 meV above the valence band.     

A pilot study for the statistical treatment of nutritional parameters in the quality control of canned fishing goods.

This pilot study was derived as a consequence of European Directives 496/90 and 493/91 in which a regulation on the labeling of canned fishing goods was established. The study was intended primarily to assess whether different Spanish canned fishing goods might be differentiated by their basic nutritional composition (i.e., ash, chlorine as NaCl, fat, humidity, total proteins, and dry residue) and, second, to study each particular type of good. Accordingly, a univariate nonparametric statistical test and 2 multivariate chemometric techniques (factor and cluster analyses) were used. The pilot study revealed that (1) the basic nutritional variables did not allow a clear distinction among canned goods when different commodities were considered, but they seemed useful for obtaining information for only one type of good; and (2) the variables that gave the most useful information to visualize the appearance of groups in the data sets were humidity, dry residue, fat, and proteins, although their particular usefulness was found to be different when different species were considered.     

catena-Poly­[[di­aqua(1,10-phen­anthroline-N,N′)­manganese(II)]-μ-(thiosulfato-O:S)] and bis(2,2′-bipyridyl-N,N′)(tetra­thionato-O,O′)manganese(II)

The structures of [Mn(S₂O₃)₂(C₁₂H₈N₂)(H₂O)₂] and [Mn(S₄O₆)(C₁₀H₈N₂)₂] are presented. The former consists of pairs of polymeric chains formed by manganese polyhedra bridged by bidentate thio­sulfate anions, which are in turn related to each other by a pseudo-twofold screw axis. The latter has crystallographic twofold symmetry and consists of monomers in which manganese displays its typical octahedral coordination provided by the bidentate bites of two bi­pyridine bases and a tetra­thionate anion, which is, to our knowledge, the first chelating tetra­thionate to be reported in the literature.     

The alternative Daugavet property of C *‐algebras and JB *‐triples

A Banach space X is said to have the alternative Daugavet property if for every (bounded and linear) rank‐one operator T: X → X there exists a modulus one scalar ω such that ∥Id+ωT ∥ = 1 + ∥T ∥. We give geometric characterizations of this property in the setting of C *‐algebras, JB *‐triples, and of their isometric preduals. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)