研究生参与实验室大型仪器管理的探索

阐述了研究生参与大型仪器管理的必要性、运行机制及实施环节,建立了"统一管理,专人负责,用管结合,开放使用"的管理模式.实践证明,这一措施的实施对规范大型仪器管理、提高仪器利用率以及实验室科研项目顺利进行起到了积极促进作用.     

三氟化硼乙醚催化合成1-(氨基甲酰基甲基)-2-烃基-3,1-苯并噁嗪类化合物

研究了三氟化硼乙醚(BF₃·OEt₂)催化2-(N-取代氨基甲酰基甲基氨基)苯甲醇与醛的反应,发展了合成取代3,1-苯并噁嗪类化合物的方法,通过该方法合成了一系列新型结构的1-(氨基甲酰基甲基)-2-烃基-3,1-苯并噁嗪类化合物。 对于这类反应BF₃·OEt₂比三甲基氯硅烷(TMSCl)和四氯化锡(SnCl₄)的普适性更广,它能有效催化这类反应,而后二者却不能。 探讨了TMSCl和SnCl₄不能催化2-(N-取代氨基甲酰甲基氨基)苯甲醇与醛反应的原因。     

Peptide dendrimer-crosslinked inorganic-organic hybrid supramolecular hydrogel for efficient anti-biofouling

A novel kind of inorganic-organic hybrid supramolecular hydrogel with excellent anti-biofouling capability was developed. The hydrogel was formed via ionic interaction between the negative-charged sodium polyacrylate (SPA) entwined clay nanosheets (CNS) and positive-charged polyhedral oligomeric silsesquioxane (POSS) core-based generation one (L-Arginine) dendrimer (POSS-R).     

Hierarchical MoS2@TiO2 Heterojunctions for Enhanced Photocatalytic Performance and Electrocatalytic Hydrogen Evolution

Hierarchical MoS₂@TiO₂ heterojunctions were synthesized through a one‐step hydrothermal method by using protonic titanate nanosheets as the precursor. The TiO₂ nanosheets prevent the aggregation of MoS₂ and promote the carrier transfer efficiency, and thus enhance the photocatalytic and electrocatalytic activity of the nanostructured MoS₂. The obtained MoS₂@TiO₂ has significantly enhanced photocatalytic activity in the degradation of rhodamine B (over 5.2 times compared with pure MoS₂) and acetone (over 2.8 times compared with pure MoS₂). MoS₂@TiO₂ is also beneficial for electrocatalytic hydrogen evolution (26 times compared with pure MoS₂, based on the cathodic current density). This work offers a promising way to prevent the self‐aggregation of MoS₂ and provides a new insight for the design of heterojunctions for materials with lattice mismatches.     

Palladium-catalyzed desulfitative arylation of sulfonamides with sodium arylsulfinates

A Pd(II)-catalyzed desulfitative arylation protocol between sulfonamides and sodium arylsulfinates was herein reported. The direct arylation reaction was successfully achieved by a Pd(II)/Ag(I)-mediated system without participation of any external ligands with a release of SO₂. And different N-aryl sulfonamides were obtained readily in up to 86% yields, exhibiting good functional groups tolerance (25 examples).     

Synthesis,crystal structures and DNA/human serum albumin binding of ternary Cu(II) complexes containing amino acids and 6‐(pyrazin‐2‐yl)‐1,3,5‐triazine‐2,4‐diamino

Two water‐soluble 6‐(pyrazin‐2‐yl)‐1,3,5‐triazine‐2,4‐diamino (pzta)‐based Cu(II) complexes, namely [Cu(l ‐Val)(pzta)(H₂O)]ClO₄ ( 1 ) and [Cu(l ‐Thr)(pzta)(H₂O)]ClO₄ ( 2 ) (l ‐Val: l ‐valinate; l ‐Thr: l ‐threoninate), were synthesized and characterized using elemental analyses, molar conductance measurements, spectroscopic methods and single‐crystal X‐ray diffraction. The results indicated that the molecular structures of the complexes are five‐coordinated and show a distorted square‐pyramidal geometry, in which the central copper ions are coordinated to N,N atoms of pzta and N,O atoms of amino acids. The interactions of the complexes with DNA were investigated using electronic absorption, competitive fluorescence titration, circular dichroism and viscosity measurements. These studies confirmed that the complexes bind to DNA through a groove binding mode with certain affinities (K_b = 4.71 × 10³ and 1.98 × 10³ M^?1 for 1 and 2 , respectively). The human serum albumin (HSA) binding properties of the complexes were also evaluated using fluorescence and synchronous fluorescence spectroscopies, indicating that the complexes could quench the intrinsic fluorescence of HSA in a static quenching process. The relevant thermodynamic parameters revealed the involvement of van der Waals forces and hydrogen bonds in the formation of complex–HSA systems. Finally, molecular docking technology was also used to further verify the interactions of the complexes with DNA/HSA.     

一种新型C60-硫醚衍生物分子在金表面上的自组装

报导了一种新型C60 硫醚分子在金表面上自组装膜的形成,并通过接触角、扫描隧道显微术（STM）、X射线光电子能谱（XPS）、电化学和光电化学手段对其进行表征.高分辩STM形貌图证明,在Au(111)基底上C60基团存在并直观显示出特殊的单层膜结构. XPS分析表明,这一新型C60 硫醚分子是通过金硫键固定在金表面上的,并且在组装过程中存在分子内碳硫键断裂步骤.     

酪氨酸、脯氨酸和组氨酸的示波极谱连续测定

提出了用示波极谱法连续测定酪氨酸 ( Tyr)、脯氨酸 ( Pro)、组氨酸( His) 3种氨基酸的新方法。在 p H9.2硼酸缓冲溶液中 ,上述 3种氨基酸与镍发生配位反应 ,用示波极谱仪进行单扫描时 ,出现 3组灵敏度和分辨率均很高的二阶导数波谱 ,峰电位分别为 :Tyr - 1 .0 4 V,Pro - 1 .2 0 V,His - 1 .34V。酪氨酸、脯氨酸、组氨酸的峰电流与浓度分别在 2 .0× 1 0 -5～ 3.0× 1 0 -4 mol/L,3.2× 1 0 -6～ 2 .2× 1 0 -4 mol/L,4.0× 1 0 -5～ 2 .5× 1 0 -4 mol/L的范围内呈线性关系。该法已用于复方氨基酸注射液中酪氨酸、脯氨酸、组氨酸含量的测定。     

毛细管气相色谱法测定面粉中的过氧化苯甲酰

采用毛细管气相色谱法测定面粉中过氧化苯甲酰的含量。方法的线性范围为0.0-500.0μg/mL,检出限为1.0ng,RSD为0.564%-0.906%,回收率为92.7%-101.3%。该法可用于面粉质量的监测。     

电感耦合等离子体光谱法测定高纯镓中的痕量元素

比较了乙醚和甲基异丁基酮（MIBK）两种萃取剂对高纯镓中基体与杂质的分离效果。选择MIBK作为萃取剂,将高纯镓中的基体元素镓萃入有机相,绝大多数金属杂质则留在水相中,用电感耦合等离子体发射光谱法测定了水溶液中 的14种痕量元素。方法的加标回收率为805－110％,检出限在0.001-0.075ug/mL之间。