质谱技术在金属配合物研究中的应用进展

综述了质谱技术的原理及质谱技术在金属配合物研究中的各种应用,通过介绍金属配合物的表征、稳定性、反应过程及研究其质谱裂解规律等几方面的应用进行了概述。     

Analysis of nisin A,nisin Z and their degradation products by LCMS/MS

The peptides nisin A and nisin Z belong to type-A lantibiotics applied as preservatives in cheese production. The present study optimised and validated a liquid chromatography–tandem mass spectrometry (LCMS/MS) method for the analysis of nisin A in cheese. Since nisin A was not detectable in nisin-containing commercial cheese samples, an additional LCMS/MS method for the quantification of nisin Z was developed and validated. Quantification was performed by external calibration and standard addition. The latter method provided a non-significantly higher recovery rate for the tested cheese matrix. During the production of processed cheese, nisin A and nisin Z undergo significant degradation. Six degradation products of nisin A or nisin Z, respectively, were detected and assigned to nisin A/Z + H₂O, nisin A/Z^1–32, and nisin A/Z^1–32 + H₂O. In two out of eight commercial processed cheese samples, 1.6, resp. 1.7 mg nisin Z/kg cheese was measured, whereas nisin A was not detectable in any of the samples.     

Analytical TEM study of annealed nanocrystalline cobalt–phosphorous electrodeposits

Investigation of thermal stability of two nanocrystalline Co–P alloys shows that P atoms segregate to the grain boundaries upon annealing until precipitation of Co₂P and CoP precipitates takes place. The P-rich precipitates formed have been investigated by analytical transmission electron microscopy to obtain statistical results of precipitate size, volume fraction and spatial distribution. Electron spectroscopic imaging maps show that the P-rich precipitates are 33 ± 9 nm in Co–1.1at.%P and 33 ± 12 nm in Co–3.2at.%P. The main differences between the alloys are the precipitate size distribution (Co–3.2at.%P having broader distribution) and precipitate volume number density (Co–3.2at.%P has 1.8 times more precipitates than Co–1.1at.%P). The volume fraction of precipitates is 3.0% in Co–1.1at.%P and 4.4% in Co–1.1at.%P. Most of the precipitates are of nearly spherical or slightly elongated shape, and only a few have a platelet-like shape as expected from previous tomographic atom probe measurements. Due to the truncation and projection effects, the composition of the precipitates could not be determined.     

芴基荧光聚合物材料合成中间体的质谱分析

本文报导了新化合物 2 ,7-双 ( 4,4 ,5 ,5 -四甲基 -1 ,3 ,2二氧杂硼烷 -二基 ) -9,9-二辛基芴的 EI和 ESI的质谱 ,利用质谱 -质谱 ( MS/ MS)分析 ,确认了该谱图中母离子和子离子的关系 ,讨论了其碎裂途径 ,为其结构鉴定提供了依据     

新型静电离子导入器的研制

A novel electrostatic ion guide(EIG) was designed and manufactured according to the simion simulation. Favorable focusing effect with high transmission efficiency was achieved by optimizing different parameters. EIG was used to ensure the vacuum difference between electrospray ionization(ESI) and time of flight mass spectrometry(TOF MS), and achieve ion-neutral molecular separation as well.     

Structural identification of a new acetildenafil analogue from pre-mixed bulk powder intended as a dietary supplement

An analogue of acetildenafil was detected in an extract of pre-mixed bulk powder. To our knowledge, the powder was destined to be encapsulated and sold as a dietary supplement. The structure was identified by NMR, HR-ESI-MS, ESI-MSⁿ and FTIR analyses. Owing to the inclusion of a hydroxyl group in acetildenafil, the detected compound was called 'hydroxyacetildenafil'. With increasing use of dietary supplements marketed for penile erectile dysfunction, the detection of analogues of sexual performance enhancers is important and timely.     

A study of Si-L and O-K ELNES in plant material: SiO2, Ca- and Zn-silicate in Minuartia

The formation of vacuolar precipitates containing silicon and calcium, as well as the accumulation of metal-silicates in cell walls of Minuartia has been investigated by electron microscopy, energy-dispersive X-ray analysis and electron spectroscopic imaging. The bond state of the elements concerned is examined by analysing energy-loss near-edge structures (ELNES), particularly the Si-L_2,3 and the O-K ELNES. Experimental ELNES results are compared with local densities of unoccupied states calculated by molecular orbital methods and results of XANES calculations.     

The ion funnel: Theory,implementations, and applications

The electrodynamic ion funnel has enabled the manipulation and focusing of ions in a pressure regime (0.1–30 Torr) that has challenged traditional approaches, and provided the basis for much greater mass spectrometer ion transmission efficiencies. The initial ion funnel implementations aimed to efficiently capture ions in the expanding gas jet of an electrospray ionization interface and radially focus them for efficient transfer through a conductance limiting orifice. We review the improvements in fundamental understanding of ion motion in ion funnels, the evolution in its implementations that have brought the ion funnel to its current state of refinement, as well as applications of the ion funnel for purposes such as ion trapping, ion cooling, low pressure electrospray, and ion mobility spectrometry. © 2009 Wiley Periodicals, Inc., Mass Spec Rev 29:294–312, 2010     

Naturally-occurring folates in foods: Method development and analysis using liquid chromatography–tandem mass spectrometry (LC–MS/MS)

An accurate method for detecting and quantifying both synthetic (folic acid) and naturally-occurring folates in foods is described. A system capable of analysing the five most commonly occurring folates (pteroylglutamic acid, 5-methyltetrahydrofolate, tetrahydrofolate, 10-formylfolate and 5-formyltetrahydrofolate) in 20 min using liquid chromatography–tandem mass spectrometry (LC–MS/MS) was developed. Quantification of folates was performed using ¹³C labelled internal standards. This paper outlines the development of a comparatively fast LC–MS/MS method, method validation using commercially available folate standards and establishment of the method’s suitability for quantification using selected reaction monitoring (SRM) mass spectrometry. The application of the system was verified by analysing several certified reference materials and comparing results with certified values as determined by microbiological assay. LC–MS/MS promises to be an ideal tool for the quantitative analysis of folates in food.