An ultrathin film of gold was grafted on human hair by a chemical liquid deposition method under ambient conditions. The method consisted of the assembling of gold nanoparticles (GNPs) on the adsorptive sites of human hair as seeds and the growth of isolated GNP seeds into a continuous gold layer. The resulting gold film coated hair possessed good conductivity and flexibility, and can be used as a novel gold hair microelectrode (GHME). This electrode inherited some merits of both hair and gold nanoparticles, for instance, good mechanical property, excellent biocompatibility and high surface area. GHME was also proven to exhibit sensitive electrochemical responses toward dopamine and nitric oxide, foreseeing its promising applications in the fields of biomedical analysis.

A novel amperometric nitric oxide sensor based on poly(eosin b)-ionic liquid composite (PEB-IL) films was described. Conducting PEB was firstly electrodeposited on the surface of a glassy carbon electrode, and then a composite of 1-hexyl-3-methylimidazolium hexafluorophosphate (HIMIMPF6) and didodecyl dimethyl ammonium bromide (DDAB) was coated on the PEB film. The resulting PEB-IL composite has the advantages of fast response and high selectivity for the determination of nitric oxide. Cyclic voltammetry (CV) and amperometric methods were employed to study the electrochemical behavior of the PEB film electrode and its electrochemical response toward NO. The results showed that the PEB-IL composite modified electrode exhibited an excellent anti-interference ability and a wide linear relationship over a NO concentration range of 3.6 × 10−8 to 1.3 × 10−4 mol/L with a low detection limit of 1.8 × 10−8 mol/L (S/N = 3). This sensor was successfully applied to the monitoring of NO release in rat kidney.

We report a simple strategy for fabricating a thin-film filtering membrane electrode (FME) of single-walled carbon nanotubes (SWCNTs) by vacuum filtration. A SWCNT–FME, comprised of SWCNTs and mixed cellulose ester (MCE), is applicable in two detection modes. The face-mode SWCNT–FME directly employs the exposed SWCNT sensing layer and possesses remarkable properties as thin-film electrochemical sensor platforms, including good flexibility, wide potential window, large surface area and excellent analytical performance resembling traditional carbon nanotube-based electrochemical sensors. The back-mode SWCNT–FME has a tunable selectivity produced by combining the separation function of the outer MCE membrane with the high surface area of the inner SWCNT sensing layer. As an example of surface functionalization, an electrodeposition method was proposed for the controlled decoration of a SWCNT–FME with either low-density discrete flower-like gold nanoparticles (GNPs) or continuous GNP films. The resulting SWCNT–GNP composites were proved to possess high surface area and excellent electrocatalytic activity for the oxidation of glucose.

The structure of cyclic aryl thioether ether sulfone oligomers was characterized by MALDI-TOF-MS. Four kinds of matrix were compared and the results showed that 1,8,9-dithranol was the effective matrix. The effect of metal cationization agents on this kind of novel aromatic cyclic oligomers was studied and silver trifluoracetate was considered as a suitable cationization agent.

鹿茸是指马鹿(Cervus elaphus Linnaeus)和梅花鹿(Cervus Nippon Temminck)未骨化的角组织,其生长极为迅速.每年都经历生长、钙化、脱落的周期性变化.鹿茸产自长白山,是著名中药材,中医临床将鹿茸作为强壮药,主要用于全身衰弱、年老或久病体虚及病后恢复期.大量研究结果证明,鹿茸中含有多种生物活性物质,能够促进机体的生长发育和新陈代谢,增强机体的免疫功能[1].本工作拟对马鹿茸中活性物质进行提取与有效成分的分离,将分离获得的马鹿茸所特有的多肽类物质采用基质辅助激光解吸飞行时间质谱(MALDI-TOFMS)技术[2]检测分子质量和纯度,采用三种常用的基质作比较,同时考察样品浓度、激光能量对其分析结果的影响.

Cyclic ether ketone oligomers containing phenolphthalein moiety were prepared via the nucleophilic substitution reaction under pseudo high dilution conditions. The structures of cyclic aryl ether ketone were determined by using the technique of matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF-MS).

本文简述了激光解吸电离飞行时间质谱(MALDI-TOF-MS)技术及其应用,同时介绍了MALDI-TDF-MS的构造、原理及特点.

A modified pseudo-high-dilution technique has been developed to synthesize phenyl-capped trianiline and tetraaniline. The reaction mechanism involved the hydrolysis of Schiff bases and their subsequent coupling reaction with diphenylamine. The products were characterized by infrared spectroscopy. MALDI-mass spectrometry, and nuclear magnetic resonance spectroscopy.

Phenyl/hydroxyl end-capped trianiline and 2-hydroxylethylamine end-capped trianiline were synthesized through simple oxidative coupling reaction. The phenyl/hydroxyl end-capped trianiline was characterized by nuclear magnetic resonance spectra, while 2-hydroxyethylamine end-capped trianiline was characterized differential scanning calorimetry to measure the melting point. The oxidative coupling method was more easy to implement as compared with traditional organic method.

Monodisperse phenyl-capped aniline pentamer and hexamer were synthesized through an oxidative coupling reaction and were characterized by infrared spectroscopy, nuclear magnetic resonance spectroscopy, MALDI-mass spectrometry and elemental analysis. The reaction mechanism seemed to involve the formation of cation radicals and their coupling reaction. The effect of chain length on the excitonic peak (λ max) was found to be different from that in the phenyl-capped polyaniline oligomers and parent aniline oligomers. Terminal groups had effects on λ max and possibly also on the conductivity. The synthesis of higher phenyl-capped oligomers was hypothesized to lead to higher conductivity.

采用基质辅助激光解吸电离飞行时间质谱(MALDI-TOF-MS)技术分别对2种合成的聚芳醚酮环状低聚物进行了分析研究,并讨论了低聚物中不同聚合度离子组分的分布规律.实验结果表明MALDI-TOF-MS是分析环状低聚物直观、准确、快速的分析工具.

Several specific non-covalent protein complexes were successfully observed by matrix assisted desorption ionization mass spectrometry(MALDI MS). The methods described in this paper include the matrixes use of sinapinic acid(SA) and 6-aza-2-thiothymine (ATT) in neutral pH solution, as well as the improvement of two-layer sample preparation method to achieve a high sensitivity detection of stable non-covalent complexes, Myoglobin-heme complex was found simultaneously with the sinapinic acid matrix in the various pH solution(pH=2 or pH=5), The RNase S complex showed a striking intensity at the first shot, which was decreased with more laser shots. Most importantly, the observation of specific non-covalent complex in the brome mosaic virus(BMV) coat proteins would open up a new possibility to investigate the assembly and disassembly of viral capsids.

The chemical and electrochemical oxidation of phenyl-capped aniline tetramer, pentamer and hexamer were studied using ultraviolet spectroscopy and cyclic voltammetry (CV). The UV spectra of the oligomers showed two broad absorptions, with the first one associated with a π-π* transition of the conjugated ring system, and with the second assigned to the benzenoid to quinoid excitonic transition. The CV of the tetramer and pentamer displayed two oxidative waves, while the CV of the hexamer showed three oxidative waves.

The mass spectrometric dissociation feature of 2,5-bis(4-hydroxybenzylidene)cyclopentanone was studied by means of tandem mass spectrometric techniques including both collision-induced dissociation and linked scan. It provides an evidence for the existence of a doubly charged ion of m/z 146. Furthermore, the collision-induced fragmentations of the doubly charged ion have been discussed.

Matrixassisted laser desorption/ionization (MALDI) mass spectra of saccharides with three common matrixes were studied here. It is shown that Na+ and K+ play important roles in the determination of oligasaccharide molecule weight and the molecular weights (MW) of glucans(dextran) with MW more than 10 000 is determined successfully with the help of column chromatography, By comparing the effects of three matrixes in saccharide analysis and comparing positive-ion and negative-ion matrixassisted laser desorption/ionization mass spectra of oligo- and polysaccharides, the most suitable matrix for saccharide analysis, 2,5-dihydroxylbezonic acid (DHB), is selected and the ion formation processes of saccharides under matrix-assisted laser adsorption/ionization condition are clarified.

The macrocyclic polyarylate oligomers have been studied by matrix-assisted laser desorption ionization mass spectrometry (MALD-MS) and the existence of oligomers with different degrees of polymerization (n = 1,2······8) has been proved satisfactorily. The experiment result shows that MALD-MS technique is a rapid, effective and accurate tool to determine the degree of polymerization in macrocyclic oligomers.

Matrix-assisted laser desorption ionization (MALDI) mass spectrometry is difficult for the characterization of noncovalent complexes hitherto because of the limitations in acidic matrix, sample preparation, laser-induced polymerization and adduct formation with matrix. Under our experimental conditions, sinapinic acid is used as a matrix, the specific noncovalent interactions of protein with fullerenols were observed by MALDI mass spectrometry. Some mass spectrometric features, such as mass shifts, broad adduct peaks and stoichiometries, showed that the specific non-covalent complexes between protein and fullerenols have been formed at a ratio of 1 : 4 for hemoglobin-fullerenols or 1 : 1 for myoglobin-fullerenols. The results implied that fullereneols could be used to protect partly hemoglobin from decomposition in acidic media, and therefore, it is possible to realize the molecular weight determination of a quaternary protein by MALDI mass spectrometry via the addition of specific organic compound in the matrix.