Identification of putative biomarker molecules within the genus Corydalis (Papaveraceae) was pursued by combining conventional off-line sample enrichment with high-performance liquid chromatography-solid phase extraction-nuclear magnetic resonance (HPLC-SPE-NMR) based structure elucidation. Off-line reversed phase solid phase extraction (SPE) was used to enrich the desired analytes from a methanolic extract (93 mg dry weight) of a miniscule single tuber (233 mg dry weight) of C. solida. An aliquot of the SPE fraction (2.1 mg) was subjected to separation in the HPLC-SPE-NMR hyphenation. Chromatographic peaks bearing the metabolites under investigation were trapped in the SPE device in a single experiment and transferred to a 600 MHz NMR spectrometer equipped with a 30 microl cryofit insert fed into a 3 mm cryoprobe. Recorded homo- and heteronuclear 1D and 2D NMR data allowed the identification of the three analytes under investigation as protopine, allocryptopine, and N-methyl-laudanidinium acetate. The latter is a rare alkaloid, which has been isolated only once before. 相似文献
Production cross-sections of charged pions, kaons and antikaons have been measured in C+C and C+Au collisions at beam energies
of 1.0 and 1.8 AGeV for different polar emission angles. The kaon and antikaon energy spectra can be described by Boltzmann
distributions whereas the pion spectra exhibit an additional enhancement at low energies. The pion multiplicity per participating
nucleon M(π+)/<Apart> is a factor of about 3 smaller in C+Au than in C+C collisions at 1.0 AGeV whereas it differs only little for the C and the
Au target at a beam energy of 1.8 AGeV. The K+ multiplicities per participating nucleon M(K+)/ <Apart> are independent of the target size at 1 AGeV and at 1.8 AGeV. The K- multiplicity per participating nucleon M(K-)/ <Apart> is reduced by a factor of about 2 in C+Au as compared to C+C collisions at 1.8 AGeV. This effect might be caused by the
absorption of antikaons in the heavy target nucleus. Transport model calculations underestimate the K-/K+ ratio for C+C collisions at 1.8 AGeV by a factor of about 4 if in-medium modifications of K-mesons are neglected.
Received: 10 December 1999 / Accepted: 14 November 2000 相似文献
The characteristics of polymer light emitting diodes (PLEDs) (ITO/PPV/Ca) depend strongly on the conditions during preparation and operation. We studied the effects of heat treatment (during and after preparation) of PLEDs with OC1C10-PPV as active layer. PLEDs showed a reduction of both the current and the light output to 40 % after annealing for only 30 min at 65 °C. Effects on I-V characteristics were studied by measuring single carrier devices (hole- and electron-dominated devices). The current reduction after heat treatment can be ascribed to degradation of the ITO/PPV and the Ca/PPV interfaces. 相似文献
Ultrashort-pulse laser ablation (τ=130 fs, λ=800 nm, repetition rate 2–20 Hz) of titanium nitride was investigated for laser
fluences between 0.3 and 4.5 J/cm2 using the direct focusing technique in air. The influence of the laser pulse number and the peak fluence was investigated
by means of several surface analytical techniques (optical microscopy, dynamic friction atomic force microscopy, scanning
Auger electron microscopy and small-spot electron spectroscopy for chemical analysis). The correlation of the results about
optical, physical and chemical properties of the irradiated areas allows us to propose a simple oxidation model, which explains
different observed phenomena associated with surface damage such as mound formation and crater widening and clarifies the
incubation behavior reported earlier for this material.
Received: 8 May 2000 / Accepted: 9 May 2000 / Published online: 13 September 2000 相似文献
CuAl2F2(Si2O7) has been prepared by hydrothermal synthesis and its crystal structure was determined by single crystal X‐ray diffraction: space group Pnma, a = 8.8697(9), b = 14.084(2), c = 4.7553(5) Å, wR2 = 0.056, R = 0.022. Cu2+ shows elongated square pyramidal coordination. Edge‐ and corner‐sharing [AlO4F2] octahedra with fluorine atoms in cis position form layers parallel to the ac plane. Along b these layers are linked by Si2O7 groups to form a three‐dimensional framework [Al2F2(Si2O7]2–. In addition, the [CuO5] pyramides connect two Al octahedra of neighbouring layers. The crystal structure is discussed as a derivative from topaz structure. The modular (or polysomatic) approach is used for this purpose, and for modelling hypothetical related compounds. 相似文献
Alkannin and shikonin (A/S) and their derivatives have been found in the roots of several Boraginaceous species and are also produced through plant tissue cultures. The chiral compounds A/S are potent pharmaceutical substances with a wide spectrum of biological and pharmacological activities like wound healing, antimicrobial, anti-inflammatory, anticancer and antioxidant activity. High-speed counter-current chromatography (HSCCC) was applied for the first time to the separation, preparative isolation and purification of A/S and their esters from extracts of Alkanna tinctoria roots, as well as commercial samples. The constituents of HSCCC fractions and their purity were determined by high-performance liquid chromatography-diode array detection-mass spectrometry (HPLC-DAD-MS), since DAD cannot detect oligomeric A/S derivatives that are present in most of the samples containing the respective monomeric derivatives. The purity of HSCCC fractions was compared with the one of fractions isolated by column chromatography (CC) using as stationary phases silica gel and Sephadex LH-20. As shown, the purity of monomeric alkannin/shikonin was greater by HSCCC than CC separation of commercial A/S samples. 相似文献
Hydroxy‐mediated methoxy formation or stabilization is probably an important process in many methanol adsorption systems. Hydrogen atoms originating from the scission of the methanol O? H bond react with the substrate and form water. This process may result 1) in the production of additional surface defects as reactive centers for methoxy formation and 2) in the stabilization of methoxy groups by suppression of methanol formation.
A novel high yield isolation procedure for lipophilic cyclic peptide derivatives is presented. Destruxin (dtx) A, B, D, E, and E-diol retrieval from Metarhizium anisopliae culture broth was achieved with a three-step purification protocol. After liquid-liquid extraction column chromatography over Sephadex LH-20 served as enrichment step. High-speed counter-current chromatography (HSCCC) was used for the final purification. Within the first chromatographic step dtx D and dtx E-diol were separated in purities exceeding 90%. The separation of dtx A, B, and E was achieved from an enriched Sephadex LH-20 fraction by a HSCCC protocol using light petroleum-ethyl acetate-methanol-water = 2:5:2:5 (v/v) as eluent system. These derivatives were obtained in purities above 98% and total yields exceeding 40%. 相似文献
A capillary electrophoresis (CE) method using non-aqueous (NA) separation solutions combined with an ion trap mass spectrometer (MS and MS/MS) as detection device is presented for the separation, identification and quantification of isoquinoline alkaloids from Fumaria officinalis. The best results were obtained with a mixture of acetonitrile-methanol (9:1, v/v) containing 60mM ammonium acetate and 2.2M acetic acid as running electrolyte and an applied voltage of 30 kV. Electrospray MS measurements were performed in the positive ionization mode with isopropanol-water (1:1, v/v) as sheath liquid at a flow rate of 3 microl/min. Alkaloids were detected as [M+H](+)-ions and showed typical fragmentation patterns in MS/MS experiments. The developed assay was used for the quantification of seven isoquinoline alkaloids representing different structural subtypes in Fumariae herba extracts and F. herba containing phytopharmaceuticals. 相似文献
The novel five-Penning-trap mass spectrometer Pentatrap is developed at the Max-Planck-Institut für Kernphysik (MPIK), Heidelberg. Ions of interest are long-lived highly charged nuclides up to bare uranium. Pentatrap aims for an accuracy of a few parts in 1012 for mass ratios of mass doublets. A physics program for Pentatrap includes Q-value measurements of β-transitions relevant for neutrino physics, stringent tests of quantum electrodynamics in the regime of extreme electric fields, and a test of special relativity. Main features of Pentatrap are an access to a source of highly charged ions, a multi-trap configuration, simultaneous measurements of frequencies, a continuous precise monitoring of magnetic field fluctuations, a fast exchange between different ions, and a highly sensitive cryogenic non-destructive detection system. This article gives a motivation for the new mass spectrometer Pentatrap, presents its experimental setup, and describes the present status. 相似文献