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111.
112.
Zanolari B Wolfender JL Guilet D Marston A Queiroz EF Paulo MQ Hostettmann K 《Journal of chromatography. A》2003,1020(1):75-89
The bark of catuaba (Erythroxylum vacciniifolium Martius, Erythroxylaceae), a tree native to the northern part of Brazil, was investigated for its alkaloid content. With the aim of obtaining preliminary structure information on-line, the alkaloid extract was analysed by high-performance liquid chromatography coupled to diode array UV detection, to mass spectrometry and to nuclear magnetic resonance. Interpretation of on-line spectroscopic data obtained from this extract led to structural elucidation of six new alkaloids and partial identification of 18 potentially original alkaloids bearing the same tropane skeleton esterified in positions 3 and 6 by 1-methyl-1H-pyrrol-2-carboxylic acid and/or 4-hydroxy-3,5-dimethoxybenzoic acid. 相似文献
113.
TA-MS provides chemical and thermal response information. In order for this information to be meaningful sampling must be
performed with minimum dead volume and without cold spots. Dead volume leads to response lag and peak broadening. Cold spots
result in sample condensation, leading to inaccurate data and potentially inlet blockage. This paper describes a hot zone
inlet system and 'in-situ' probe both of which provide fast response, zero dead volume sampling directly to the MS. The paper
also discusses data interpretation methodologies and introduces 'soft ionisation' as a means of providing simplified analysis
of complex mixtures.
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献
114.
质谱在肽和蛋白质序列分析中的应用 总被引:7,自引:0,他引:7
了解肽和蛋白质的序列对理解其功能具有重要意义,测定其序列也是当前生命 科学研究中的重要内容之一,质谱作为高灵敏度的测定分子结构的仪器,其高灵敏 度、广泛的适用性及快速性等特性使它具有很大潜力发展成为辅助传统测序方法的 新方法,并得到了广泛的关注。从离子活化方法(包括碰撞诱导解离CID、源后裂 解PSD、源内裂解ISD等)、衍生化作用以及氨基酸残基消除方式(高能活化产生亚 稳离子、化学降解、酶降解)等多个角度介绍了利用质谱分析多肽和蛋白质序列的 方法,并对其发展前景作出展望。 相似文献
115.
Glassy carbon electrodes modified with (5-amino-1,10-phenanthroline)bis(bipyridine)ruthium(II) chloride hydrate, [(bpy)2Ru(5-phenNH2)]Cl2·H2O, are shown to oxidize hydrazine with excellent sensitivity. The presence of an amine group on the ruthenium complex facilitates electropolymerization onto the electrode surface. Using cyclic voltammetry, a large catalytic current is observed upon oxidation of hydrazine in phosphate buffer (pH 5.0), compared to the current obtained from the ruthenium-modified electrode with no hydrazine present. The sensitivity of cyclic voltammetry is sufficient for obtaining a linear calibration curve for hydrazine over the range of 10−5 to 10−2 M. Hydrodynamic amperometry was used to determine the working potential for flow injection analysis. The limit of detection for hydrazine was determined to be 8.5 μM using FIA. The thickness of these films was shown to increase linearly with the number of electropolymerization cycles, in the range of 1000-2500 nm for 5-20 cycles, respectively, using Rutherford backscattering spectrometry (RBS). RBS analysis also suggests that the film is multilayered with the outermost layers containing a high ruthenium concentration, followed by layers where the concentration of ruthenium decreases linearly and approaches zero at the electrode surface. 相似文献
116.
A method for the preconcentration of gold in natural waters at the sampling site using tributyl phosphate as a solid extractant [Se(TBP)] was developed as a preliminary step prior to the determination of gold by neutron activation and γ-spectrometry. The SE(TBP) was saturated with gaseous chlorine for extracting all gold species. In batch experiments gold was quantitatively retained on the SE(TBP) in 10 min. After extraction and washing, the SE(TBP) was ashed or back-extracted. Gold was quantitatively eluted with hot, neutral 0.025 M thiourea. The gold content of residues of ashing or eluents after evaporation was determined by neutron activation and γ-spectrometry. The detection limit for the overall procedure was 0.2 ng 1?1. The efficiency was tested on ‘equilibrated’ solutions prepared from river water and tracer solutions of gold. For comparison, the gold content of natural water samples was determined using preconcentration on activated charcoal. 相似文献
117.
E.?BertoloEmail author J.?A.?Kilner M.?Sahibzada 《Journal of Solid State Electrochemistry》2004,8(9):585-591
18O/16O isotope exchange depth profiling (IEDP) combined with secondary ion mass spectrometry (SIMS) has been used to measure the oxygen tracer diffusivity of SrCe0.95Yb0.05O3– between 800 °C and 500 °C at a nominal pressure of 200 mbar. The values of D* (oxygen tracer diffusion coefficient) and k (surface exchange coefficient) increase steadily with increasing temperature, and the activation energies are 1.13 eV and 0.96 eV, respectively. Oxygen ion conductivities have been calculated using the Nernst–Einstein equation. The transport number for oxide ions at 769 °C, the highest temperature studied, is only ~0.05. Moreover, SrCe0.95Yb0.05O3– has been studied using impedance spectroscopy under dry O2, wet O2 and wet H2 (N2/10% H2) atmospheres, over the range 850–300 °C. Above ~550 °C, SrCe0.95Yb0.05O3– shows higher conductivity in dry O2 than in wet O2 or wet H2; below that temperature the results obtained for the three atmospheres are comparable. Dry O2 shows the highest activation energy (0.77 eV); the activation energies for wet O2 and wet H2 are identical (0.62 eV).Abbreviations HTPC high-temperature proton conductor - IEDP isotope exchange depth profiling - SIMS secondary ion mass spectrometryPresented at the OSSEP Workshop Ionic and Mixed Conductors: Methods and Processes, Aveiro, Portugal, 10–12 April 2003 相似文献
118.
This document reviews the most relevant mass spectrometry approaches to selenium (Se) speciation in high-Se food supplements in terms of qualitative and quantitative Se speciation and Se-containing species identification, with special reference to high-Se yeast, garlic, onions and Brazil nuts. Important topics such as complexity of Se speciation in these materials and the importance of combining Se-specific detection and molecule-specific determination of the particular species of this element in parallel with chromatography, to understand their nutritional role and cancer preventive properties are critically discussed throughout. The versatility and potential of mass spectrometric detection in this field are clearly demonstrated. Although great advances have been achieved, further developments are required, especially if speciatedcertified reference materials (CRMs) are to be produced for validation of measurements of target Se-containing species in Se-food supplements. 相似文献
119.
建立了超高效液相色谱-三重四极杆质谱联用技术测定血浆和尿液中马桑中毒标志物马桑亭和马桑宁的方法。血浆和尿液样品经固相支持液液萃取法提取净化后,溶于15%(v/v)甲醇水溶液中,以Cortecs C18色谱柱(100 mm×2.1 mm,1.6 μm)作为分析柱进行分离,电喷雾负离子多反应监测(MRM)模式下检测,以氟苯尼考作为内标物,基质工作曲线内标法定量。血浆和尿液中马桑亭和马桑宁的平均加标回收率为86.2%~110%,相对标准偏差为5.1%~14.6%(n=6),血浆中马桑亭和马桑宁的检出限(S/N=3)分别为0.01 μg/L和0.1 μg/L,尿液中马桑亭和马桑宁的检出限分别为0.03 μg/L和0.3 μg/L。本法简单、灵敏、准确,可用于血浆和尿液中马桑亭和马桑宁的中毒检测。 相似文献
120.
石墨炉原子吸收光谱无标样分析法的研究:Ⅰ.消除基体干扰 总被引:1,自引:0,他引:1
实现石墨炉原子吸收光谱绝对分析必须消除基体干扰,本研究采用有机基体改进剂,管壁原子化、热解涂层石墨管,峰面积积分吸收信号,D2灯或Zeeman效应扣除背景,有效地控制和消除了海水基体对As,Cd,Co,Cr,Cu,Mn,Ni,Pb和V等元素的干扰,实现了无干扰测定。 相似文献