Counterexamples to a conjecture of mader about cycles through specified vertices inn-edge-connected graphs

For each oddn≥3, we constructn-edge-connected graphsG with the following property: There are two verticesu andv inG such that for every cycleC inG passign throughu andv the graphG-E(C) is not (n-2)-edge-connected. HereE(C) denotes the set of edges ofC, and a cycle is allowed to pass through a vertex more than once.     

Katalytische Oxidation von NADH an Graphitelektroden durch adsorbierte Phenoxazinderivate

Zusammenfassung Phenoxazin und 2-Naphthoylderivate von Aminophenoxazinen wie Nilblau (E ₀=–220 mV/SCE bei pH 7) wurden an Graphitelektroden adsorbiert. Diese Substanzen sind sehr gute Katalysatoren zur NADH Oxidation zu NAD⁺, wenn ihr Redoxpotential nicht unter –300mV/SCE liegt. Die Vergrößerung des Moleküls durch die Napthoylgruppe oder die Benzolringe kondensierter Polyaromaten als zusätzliche Haftgruppen setzt ihre Löslichkeit in wäßrigen Lösungen stark herab. Auf Graphit kann 2-Naphthoylnilblau bis pH 8 benützt werden, bei größeren pH-Werten hat es durch die Umwandlung in seine Iminoform eine geringere Aktivität. In Lösung ist die Iminoform vollständig inaktiv. Es wird angenommen, daß die Reaktion über einen Charge-Transfer-Komplex verläuft, ohne daß ungebundene Elektronen und Wasserstoff freigesetzt werden (H^– in der Gesamtreaktion).

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Catalytic oxidation of NADH on graphite electrodes with adsorbed phenoxazine derivates

Summary Phenoxazines and 2-naphthoyl derivates of aminophenoxazines like Nilblue (E ₀=–220mV/SCE at pH 7) had been adsorbed on graphite electrodes. These substances are very good catalysts for NADH oxidation to NAD⁺, if their redox potential is not under –300 mV/SCE. The enlargement of the molecule by the naphthoyl group or by the benzene rings of condensed polyaromatics as additional adhesive group very strongly lower their solubility in aqueous solutions. 2-Naphthoyl nilblue can be used up to pH 8, in case of higher pH values it has a lower activity due to its conversion into the imino form. In solution the imino form is completely inactive. It is suggested that the reaction involves a charge-transfer complex without releasing unbound electrons and hydrogen (H^– in the overall reaction).

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Diese Arbeit wurde vom Bundesministerium für Forschung und Technologie unterstützt. Herrn Prof. H.-L. Schmidt danke ich für die Förderung dieser Arbeit.     

Beta decay of the MT=-1 nucleus 58Zn studied by selective laser ionization

Beta decay of ⁵⁸Zn has been studied for the first time. A new laser ion-source concept has been used to produce mass-separated sources for beta and gamma spectroscopy. The half-life of ⁵⁸Zn was determined to be 86(18) ms. Comparisons are made with previous data from charge-exchange reactions. Our Gamow–Teller strength to the 1⁺ state at 1051 keV excitation in ⁵⁸Cu agrees well with the value extracted from a recent (³He, t) study. Extensive shell-model calculations are presented. Received: 5 June 1998 / Revised version: 24 July 1998     

Homogeneity examination of a disordered magnetic alloy by means of CEMS

The depth sensitivity of the Mössbauer effect conversion electron spectroscopy (CEMS) offers a possibility to check the homogeneity of an alloy as a function of the sample thickness. We present experimental results on (Fe_0.65Ni_0.35)_1-xMn_x (x=0.026) prepared by diffusion of Mn into a Fe_0.65Ni_0.35 foil. On an inhomogeneous sample we determined the diffusion coefficient of Mn in Fe_0.65Ni_0.35 at 1300 K to be about 10^?11 cm²/s.     

TheN=83 nucleus149Dy from Gamow-Teller decay of its 11/2− and 1/2+ 149Ho parents

A high-sensitivityγ-spectroscopic study of the¹⁴⁹Hoπh _11/2 andπs _1/2 β-decays using mass separated sources has located dominant 0⁺ → 1⁺ GT decay strength associated with decay of pairedh _11/2 protons, leading to 3п-states in the¹⁴⁹Dy daughter nucleus. In theirγ-decay low-lying¹⁴⁹Dy levels characteristic of anN=83 nucleus are excited. They include theνf _7/2,νp _3/2,νh _9/2 andνp _1/2 single particle- and theνs ₁ ^2/?1 andνd ₃ ^2/?1 two-particle one-hole states, as well as the νf _7/2 × 3^? andνf _7/2 × 2⁺ particle-phonon multiplets. A synopsis is given of these excitations in theN=83 isotones from¹⁴⁹Nd to¹⁵³Yb. The¹⁴⁹Dy GT decay strength is discussed in terms of the¹⁴⁷Tb₈₂ and¹⁴⁸Dy₈₂ decays. The strength function results are also compared with independent¹⁴⁹Ho 11/2^? decay data from the literature based on totalγ-ray absorption measurements.     

Photoaddition of water and alcohols to the anthracene moiety of 9-(2'-hydroxyphenyl)anthracene via formal excited state intramolecular proton transfer

The title compound undergoes efficient photoaddition of a molecule of a hydroxylic solvent (H(2)O, MeOH, (Me)(2)CHOH) across the 9- and 10-positions of the anthracene moiety to give isolable triphenylmethanol or triphenylmethyl ether type products. The reaction is believed to proceed via a mechanism involving water-mediated formal excited state intramolecular proton transfer (ESIPT) from the phenolic OH to the 10-position of the anthracene ring, generating an o-quinone methide intermediate that is observable by nanosecond laser flash photolysis, and is trappable with nucleophiles. A "water-relay" mechanism for proton transfer seems plausible but cannot be proven directly with the data available. Irradiation in deuterated solvents led to incorporation of one deuterium atom at the methylene position in the photoaddition product, and partial deuterium exchange of the 10-position of recovered starting material, consistent with the proposed formal excited state proton transfer mechanism. The deuterium exchange and photoaddition reach maximum quantum efficiency at approximately 5 M water (in CH(3)CN or CH(3)OH), with no reaction observed in the absence of a hydroxylic solvent, demonstrating the sensitivity of this type of ESIPT to solvent composition.     

Isolation and characterization of methoxylated flavones in the flowers of Primula veris by liquid chromatography and mass spectrometry

Characterization of six flavones, which were named substances G1, G2, G3, G4, G5 and G6 according to their R_F values in normal-phase thin-layer chromatography, is reported. The pure flavones were purified after maceration with methanol by normal-phase solid-phase extraction, normal-phase medium-pressure liquid chromatography, normal-phase preparative thin-layer chromatography and preparative reversed-phase high-performance liquid chromatography (RP-HPLC). The collected fractions of several isolation steps were analyzed by normal-phase (NP) and RP-HPLC. Detection and identification of the substances G was accomplished by UV detection at 213–216 nm, diode array UV detection, or fluorescence detection (λ_ex=330 nm; λ_em=440 nm). The molecular mass, the elementary composition, and the structure of the six components was determined by electron-impact high-resolution mass spectrometry (EI-HRMS). Substance G4 was identified as 3′,4′,5′-trimethoxyflavone. The substances G1–G6 were shown to be mono-, di- tri- and pentamethoxyflavones. HPLC–electrospray ionization tandem mass spectrometry (ESI-MS–MS) of the flavones was carried out employing a 150×2 mm I.D. column packed with a 3 μm/100 Å octadecylsilica stationary phase and a mobile phase comprising 1.0% acetic acid in water–acetonitrile (50:50). Comparative RP-HPLC–ESI-MS of the raw methanol extract and the isolated substances G1–G6 proved that the isolated compounds were pure and were not artifacts. Finally, RP-HPLC–ESI-MS–MS was used to identify substances G1–G6 in phytopharmaceutical drugs.     

Amino-Functionalized Monolithic Poly(glycidyl methacrylate-<Emphasis Type="Italic">co</Emphasis>-divinylbenzene) Ion-Exchange Stationary Phases for the Separation of Oligonucleotides

Monolithic capillary columns were prepared by thermal initiated copolymerization of glycidyl methacrylate (GMA) and divinylbenzene (DVB) inside silanized 200 µm i.d. fused silica capillaries. Polymerization mixtures containing different amounts of porogen (1-decanol and tetrahydrofuran (THF)) and different ratios of monomer and crosslinker were used for synthesis. For characterization the pore size distribution profiles of the resulting monoliths were determined by mercury intrusion porosimetry. The morphology of the copolymer was investigated by scanning electron micrographs (SEM). A high linear dependence between flow rate and pressure drop was achieved which indicates that the polymer is pressure-stable even at high flow rates. After characterization the produced GMA-DVB monoliths, which contain reactive epoxide groups, were modified by reaction with diethylamine to obtain a poly(3-diethylamino-2-hydroxypropyl methacrylate-co-divinylbenzene) ion-exchange monolithic stationary phase. The synthesized monoliths contain ionizable amino groups that are useful for anion-exchange chromatography (AEC). Poly(3-diethylamino-2-hydroxypropyl methacrylate-co-divinylbenzene) monolithic columns allowed a fast and highly efficient separation of a homologous series of phosphorylated oligothymidylic acids [d(pT)_12-18]. Since durability is an important parameter of chromatographic column characterization, the separation performance for d(pT)_12-18 in a freshly produced capillary column and on the same column after 100 chromatographic runs was compared.     

Development and evaluation of a new method for the determination of the carotenoid content in selected vegetables by HPLC and HPLC-MS-MS

Epidemologic studies have shown inverse correlation between the consumption of carotenoid-rich vegetables and the incidence of cancer. Therefore, analytical techniques for the quantitative determination of carotenoids in complex sample matrices are important. The most used method is reversed-phase (RP)-high-performance liquid chromatography (HPLC). In this study, seventeen mobile-phase systems described in the literature and six RP-HPLC columns with differences in particle size and porosity are evaluated. Derived from these results, a new mobile-phase (acetonitrile, methanol, chloroform, and n-heptane) including solvent modifiers is presented, which allows an improved and more efficient separation of carotenoids. From all columns tested, the best chromatographic parameters are found using a silica C18 column (250 x 2 mm, 5 microm, 100 A). As was found, absorbance detection at 450 nm allows the determination of the carotenoids down to the picogram range with good linearity (R2 > 0.98). For the identification and quantitation of carotenoids in complex sample matrices (containing additionally other ultraviolet-absorbing compounds), the optimized RP chromatographic system is coupled to a mass spectrometer (MS) using an atmospheric pressure ionization interface. The calibration plots show high linearity (R2 > 0.99), and the detection limit is found in the lower nanogram range. Furthermore, collision-induced dissociation in the ion source allows for the identification of carotenoids by their characteristic fragmentation pathways. In this study, a total of nine species of vegetables commonly consumed in Central Europe are analyzed for their contents of carotenoids (namely lutein, zeaxanthin, beta-cryptoxanthin, and beta-carotene) by RP-HPLC and RP-HPLC-MS-MS. It is found that good sources for lutein are spinach, kale, and broccoli, and sources for beta-carotene are broccoli, spinach, kale, carrots, and tomatoes. This new method is an improvement for the identification and quantitation of carotenoids in complex biological tissues.