Development of core–shell structure Fe3O4@Ta2O5 microspheres for selective enrichment of phosphopeptides for mass spectrometry analysis

Protein phosphorylation is one of the most important post-translational modifications. Due to the dynamic nature and low stoichiometry of the protein phosphorylation, enrichment of phosphopeptides from proteolytic mixtures is often necessary prior to their characterization by mass spectrometry. Many metal oxides such as titanium dioxide and zirconium dioxide have been successfully applied to isolation and enrichment of phosphopeptides. Recently, niobium pentoxide was proved to have the ability for selective enrichment of phosphopeptides. Considering the proximity of tantalum to niobium, we supposed that Ta₂O₅ can be used as affinity probes for phosphopeptide enrichment. In the work, we synthesized Fe₃O₄@Ta₂O₅ magnetic microspheres with core–shell structure for selective enrichment of phosphopeptides. To demonstrate its ability for selective enrichment of phosphopeptides, we applied Fe₃O₄@Ta₂O₅ magnetic microspheres to isolation and enrichment of the phosphopeptides from tryptic digestion of standard proteins and real samples, and then the enriched peptides were analyzed by matrix-assisted laser desorption mass spectrometry analysis (MALDI-MS) or liquid chromatography coupled to electrospray ionization mass spectrometry (LC–ESI-MS). Experiment results demonstrate that Ta₂O₅ coated-magnetic microspheres show the excellent potential for selective enrichment of phosphopeptides.     

Mass transfer kinetics and breakthrough and elution curves for bovine serum albumin using cibacron blue cellulose membranes

The mass transfer of bovine serum albumin onto a stack of cibacron blue cellulose membranes in the loading and elution stages were studied. The breakthrough curves obtained in the loading stage were fitted to the pore and the lumped kinetic (LK) models, respectively. Then experimental data obtained in the elution stage were described by using the LK model in which the kinetic equation, the initial and the boundary conditions were rewritten according to the operation. For the breakthrough curves it was found that the contribution of the sorption kinetics to band broadening was significant whereas that of axial dispersion was negligible. In contrast, both of these contributions were significant to the profile of the elution curve. By studying the mass transfer kinetics in the elution stage, information about the influence of the module geometry on the performance of affinity membrane separations may be obtained.     

Development of gas chromatography-mass spectrometry following headspace single-drop microextraction and simultaneous derivatization for fast determination of short-chain aliphatic amines in water samples

In this work, for the first time, gas chromatography-mass spectrometry (GC-MS) following headspace single-drop microextraction (HS-SDME) and simultaneous derivatization was developed for fast determination of short-chain aliphatic amines (SCAAs) in water samples. In the proposed method, SCAAs in water samples were headspace extracted and concentrated by suspending a microdrop of solvent, and SCAAs extracted in the microdrop of solvent were simultaneously and rapidly reacted with pentafluorobenzaldehyde (PFBAY). The formed SCAA derivatives were analyzed by GC-MS. The HS-SDME parameters of solvent selection, solvent volume, sample temperature, extraction time and stirring rate were studied, and the method linearity, precision and detection limits, were also studied. The results show that the proposed method provided good linearity (R(2)>0.99, 5.0-500 ng/ml), low detection limit (0.6-1.1 ng/ml), and good precision (RSD value less than 10%). The proposed method was further tested by its application to quantitative analysis of SCAAs in four wastewater samples. The experiment results have demonstrated that GC-MS following HS-SDME and simultaneous derivatization is a simple, rapid and low-cost method for the determination of SCAAs in water samples.     

Embedding copper nanoparticle-anchored conductive nano-blocks in polyelectrolyte

Conductive carbon nanotubes （CNTs） or alternatively polyaniline （PANI） nano-blocks was introduced into aqueous solutions of polyvinyl alcohol （PVA） and copper （II） salt, to assist the reduction of copper （II） ions and the anchoring of the resulting copper nanoparticles onto the conductive blocks. The mixture solutions of nano-blocks, copper （lI） salts and PVA were spin-coated onto the cathode surface, forming swollen cathode films （SCFs）. The copper （II） ions in the film assembled onto the surfaces of the conductive blocks and were then reduced under an appropriate voltage. It is important that the copper nanoparticles grew only on the surfaces of the conductive blocks. PVA which acted as the matrix of the composites played a role in stabilizing the resulting copper nanoparticles. Morphologies of these polymeric composite films were studied by various characterization methods. Moreover, the mechanism of migration of copper （II） ions, the formation of these polymeric composites, and the overall procedure were investigated in detail.     

共沸蒸馏法制备表面化学改性氢氧化镁纳米颗粒

首次将表面改性剂如硬脂酸、硬脂酸锌或稀土偶联剂加入到传统的共沸蒸馏体系中,使Mg(OH)2纳米颗粒的表面改性和干燥过程同时完成。 通过 XRD、TEM、FT-IR、TG和CAM（接触角测试）等技术手段对样品的结构、形貌和性质进行了表征。 结果表明,表面改性剂不但能够和Mg(OH)2纳米颗粒的表面的OH-离子发生化学反应形成表面修饰层, 减少硬团聚现象,而且还使纳米颗粒表面由亲水性变为疏水性。 另外,对共沸蒸馏法制备表面改性纳米颗粒的机理进行了讨论,为纳米颗粒表面改性提供了一种新思路。     

钼网衬底上大面积硅纳米线的制备及其光催化性能研究

硅纳米材料广泛应用于光功能导向的各个领域,发展针对光功能应用及一维硅纳米结构的规模化可控制备方法,实现硅纳米结构的宏量制备,将为硅纳米结构的应用提供材料保障。本文采用简单的化学气相沉积法成功地在Mo网衬底上制备了大面积的硅纳米线(SiNWs),并通过扫描电子显微镜、透射电子显微镜、X射线粉末衍射仪、拉曼光谱仪,对制备的SiNWs进行了详细的研究。通过在低功率紫外光照射下SiNWs对罗丹明B和甲基蓝的光降解能力的研究,发现在Mo网衬底上生长的SiNWs对于有机染料具有很好的降解能力。     

Fe掺杂ZnO空心微球的制备与光催化性能

ZnO是一种重要的Ⅱ-Ⅵ族半导体材料,其能带宽度约为3.37eV,在光电子学、传感、光催化、发电等诸多领域都具有巨大的应用潜力。本文采用简单的离子交换和热蒸发法成功制备了Fe掺杂ZnO空心微球,并利用扫描电镜、透射电镜、X射线粉末衍射仪对其形貌、结构以及成分等进行了详细的表征。光吸收测试证明Fe元素掺杂能够扩展ZnO的光吸收波段,实现波长375~600nm的光波吸收。另外,光催化实验证明Fe掺杂ZnO空心微球能够有效地促进罗丹明B的降解,表明合成的Fe掺杂ZnO空心微球是一种优异的光催化剂。     

A highly sensitive sensor for Cu2+ with unmodified gold nanoparticles and DNAzyme by using the dynamic light scattering technique

Copper ion (Cu(2+)) plays an important role in many biological reactions, and a suitable level of Cu(2+) is necessary for the regular metabolism of life. Thus developing a sensitive and simple method for determination of Cu(2+) is essential. Here, a novel and sensitive Cu(2+) sensor was developed based on detecting the average hydrodynamic diameter of AuNPs by using dynamic light scattering (DLS). Cu(2+)-specific DNAzyme was double-strand and could not adsorb on the surface of AuNPs, accordingly AuNPs aggregation would occur with the addition of NaCl. However, Cu(2+) could cleave DNAzyme and release single-stranded DNA (ssDNA) fragments, which could adsorb on the surface of AuNPs and prevent them from aggregation. Such differences in DNA adsorption ability on AuNPs before and after the addition of Cu(2+) affected the disperse state of AuNPs directly, and then affected their average hydrodynamic diameter, which could be detected with the DLS technique. Based upon the above mentioned principle, detection of Cu(2+) could be realized over the range from 100 pM to 2.0 nM, with a linear regression equation of D = 306.73 - 89.66C (C: nM, R = 0.9953) and a detection limit of 60 pM (3δ/slope). Moreover, satisfactory results were obtained when the assay was applied in the detection of Cu(2+) in water samples.     

4(6)-{2-[4-(2,3,4-三甲氧基苄基)哌嗪-1-基]-2-氧代乙氧基}芳甲酰胍类化合物的合成及其Na~+/H~+交换器1抑制活性

NHE1(Na+/H+交换器1)抑制剂对于心肌缺血再灌注损伤具有较好的保护作用.以苯(或吡啶)甲酰胍为母核,利用拼合原理,在苯(或吡啶)甲酰胍母环上引入4-(2,3,4-三甲氧基苄基)哌嗪-1-甲基,设计并合成了8个未见文献报道的目标化合物.其结构经MS,IR,1H NMR和元素分析确证.体外血小板肿胀模型(PSA)试验结果表明,大部分目标化合物显示出较好的NHE1抑制活性.     

A selective fluorescent turn-on NIR probe for cysteine

A selective and sensitive turn-on fluorescent NIR probe for cysteine has been developed. Cleavage of 2,4-dinitrobenzenesulfonyl (DNBS) with thiols switches the weakly fluorescent aza-BODIPY dye (λ(em) = 734 nm, Φ(f) = 0.03) to a strongly fluorescent species in the NIR region (λ(em) = 755 nm, Φ(f) = 0.14).