系列线型［M_2M′S_4O_4］~（2－）簇的合成及光谱与结构的关系（M＝Mo，W；M′＝Co，Mi，Fe）

报道了６种线型簇合物［Ｅｔ_４Ｎ］_２［Ｍ_２Ｍ′Ｓ_４Ｏ_４］（Ｍ＝Ｍｏ，Ｗ；Ｍ′＝Ｃｏ，Ｎｉ，Ｆｅ）的合成，通过对ＵＶ－Ｖ_（ｉｓ）、ＩＲ及ＸＰＳ光谱的对比分析，讨论了簇阴离子［Ｍ_２Ｍ′Ｓ_４Ｏ_４］~２－中心金属Ｍ′的ｄ电子结构、氧化态以及［Ｍ′Ｓ_４］的微环境，由此推测了簇阴离子构型，并讨论了化合物的稳定性．     

等瓣置换反应的研究──手性簇合物［（η~5－MeO_2CC_5H_4）（CO）_2Mo］·［（η~5－MeO_2CC_5H_4）（CO）_2W］Fe（CO）_3（μ_3－S）的分子结构及晶体结构

用Ｘ射线衍射法测定了由η~５－ＭｅＯ_２ＣＣ_５Ｈ_４）（ＣＯ）_３ＭｏＮａ和［（η~５－ＭｅＯ_２ＣＣ_５Ｈ_４）（ＣＯ）_２Ｗ］Ｆｅ－（ＣＯ）_３Ｃｏ（Ｃｏ）_３（μ_３－Ｓ）的等瓣置换反应所生成的手性簇合物──［（η~５－ＭｅＯ_２ＣＣ_５Ｈ_４）（ＣＯ）_２Ｍｏ］－［（η~５－ＭｅＯ_２ＣＣ_５Ｈ_４）（ＣＯ）_２Ｗ］Ｆｅ（ＣＯ）_３（μ_３－Ｓ）的分子结构及晶体结构。晶体属Ｐ１空间群，晶胞参数α＝０．８７１６２（５）ｎｍ，ｂ＝０．７６２１８（４）ｎｍ，ｃ＝１．８７１１１（８）ｎｍ；α＝９４．１６４（４）°，β＝９７．９７９（２）°，γ＝９９．１０８（２）°，Ｚ＝２，μ＝５．９ｃｍ~（－１）。最终的一致性因子Ｒ＝０．０３６，Ｒｗ＝０．０３７．该簇合物含ＭｏＷＦｅＳ四面体簇核，其中Ｍｏ、Ｗ原子以１：１的比例无序地分占了四面体的２个顶点．     

［Vmo_3O_4（O_2CEt）_8］_2Na_2的合成与结构

［ＶＭｏ３Ｏ４（Ｏ２ＣＥｔ）８］２Ｎａ２（１），三斜晶系，Ｐ１空间群，ａ＝１２．９７７（７），ｂ＝１４．０７０（６），ｃ＝１２．３３８（８），α＝１０９．８１（４），β＝１１７．２０（４），γ＝９０．５１（５）°，Ｖ＝１８４８．８３，Ｍｒ＝２０２０．６，Ｄｃ＝１．８１ｇ／ｃｍ３，Ｚ＝１，Ｆ（０００），μ＝１２．９ｃｍ１（ＭｏＫα）对３７４２个可观测反射点（Ｉ＞３σ（Ｉ））最终一致性因子为Ｒ＝０．０１８，Ｒω＝０．０５４。单晶结构分析表明，簇阴离子中两个［Ｍｏ３Ｏ４］４＋单元通过两个＂桥＂金属Ｖ原子连接成一个奇特的环状结构，Ｍｏ－Ｍｏ平均键长为２．５１９（１），Ｍｏ…Ｖ间平均距离为３．６５４。簇阴离子通过Ｎａ＋连成一个一维长链，Ｎａ原子与氧原子形成一个少见的五配位三角双锥结构，Ｎａ－Ｏ距离仅为２．３１２，Ｎａ－Ｏ间较强的相互作用以及无限长链的晶体结构很好地解释了簇合物（１）的稳定性和不溶性。     

两个环己烷螺含氮杂环化合物的合成和晶体结构

环己酮与硫代碳酰肼在不同介质中的反应，合成出两个不同的环己烷螺含氮杂环化合物。经Ｘ－射线结构分析确定它们分别为１，２，４，５－四氮螺［５，５］十一烷－３－硫酮，Ｃ＿７Ｈ＿（１４）Ｎ＿４Ｓ（Ⅰ）和１，２，４，－三氮螺［４，５］癸－１－烯－４－氨基－３－硫酮。Ｃ＿７Ｈ＿（１２）Ｎ＿４Ｓ＿ｘ（Ｓ＿ｘ＝０．８Ｓ＋０．２Ｏ）（Ⅱ）。晶体学参数分别为（Ⅰ）：Ｐ２＿１／ｃ，ａ＝１２．０２６（４），ｂ＝２６．８１７（６），ｃ＝１２．０４２（３），β＝１１５．９４（２）°，Ｚ＝４，Ｖ＝９３３．４（１０），Ｍ＿ｒ＝１８６．２８；（Ⅱ）：Ｐ２＿１／ｍ，ａ＝６．５９５（７），ｂ＝６．８１７（６），ｃ＝１０．５７２（６），β＝１０６．３（１）°，Ｖ＝４５６（１），Ｚ＝２，Ｍ＿ｒ＝１８１．０５。最终一致因子分别为Ｒ＝０．０５４，Ｒ＿ｗ＝０．０６５和Ｒ＝０．０８９，Ｒ＿ｗ＝０．０９６。两个化合物中，环己烷都为椅式构型，它与其螺联的６员氮杂环，５员氮杂环的最小二乘平面间的夹角分别为６８．９４和９０°。并对合成反应途径作了初步讨论。     

FeCo2(CO)7(μ3-S)(O[P(SCH2)2]2)的合成与晶体结构

许多化学工作者对单齿膦配体（ＰＰｈ３,ＰＢｕｎ３,ＰＥｔ２Ｐｈ,Ｐ（ＯＥｔ）３,Ｐ（ＯＣ６Ｈ５）３）与母体簇合物ＦｅＣｏ２（ＣＯ）９（μ３－Ｓ）的取代反应进行过详细研究［１－３］,但对双齿膦配体与母体簇合物的取代反应研究报导较少．Ａｉｍｅ［４］合成了含双齿膦配体的簇合物ＦｅＣｏ２（ＣＯ）７（μ３－Ｓ）（Ｐｈ２ＰＣＨ２ＰＰｈ２）,并用１３ＣＮＭＲ和ＩＲ光谱方法对其结构进行了表征．到目前为止,含双齿膦配体的该类簇合物的晶体与分子结构还未见报导．ＲｏｓａｎｎａＲｏｓｓｅｔｔｉ［２］通过研究母体簇合物与…     

α－石英表面自由基和离体肺泡巨噬细胞内游离Ca~（2＋）、Mg~（2＋）浓度的关系

本文用ＡＲ－ＣＭ－ＭＩＣ阳离子测定系统及Ｆｕｒａ－２荧光技术，研究了研磨后表面存在自由基的α－石英，和离体肺泡巨噬细胞作用后细胞内游离Ｃａ２＋浓度（［Ｃａ２＋］）和游离Ｍｇ２＋浓度（［Ｍｇ２＋］ｉ）的关系．发现在含Ｃａ２＋和Ｍｇ２＋的介质中，α－石英表面自由基越多，［Ｃａ２＋］ｉ和［Ｍｇ２＋］ｉ升高越大；在无Ｃａ２＋和Ｍｇ２＋的介质中，新研磨的α－石英能引起［Ｃａ２＋］ｉ和［Ｍｇ２＋］ｉ升高．Ｃａ２＋和Ｍｇ２＋的升高可能部分由于细胞内结合钙和结合镁的释放．     

二苯并（b,f）（1,4）氧杂吖庚因在银胶体系中产生SERS的机理探讨

通过滴加ＮａＮＯ３、ＮａＯＨ、ＨＮＯ３、Ｈ２ＳＯ４和ＨＣｌ对银胶体系及ＣＲ（二苯并［ｂ，ｆ］［１，４］氧杂吖庚因）ＳＥＲＳ（表面增强喇曼散射）信号的影响，探讨滴加酸溶液引起银胶体系中ＣＲ瞬即产生ＳＥＲＳ的机理。     

含MoFe3Se4类立方烷核芯簇合物的合成与结构表征

室温下［Ｅｔ_４Ｎ］_２ＭｏＳｅ_４, ＦｅＣｌ_２和 Ｒ_２ＮＣＳ_２Ｎａ在 ＤＭＦ和 ＣＨ_３ＣＮ混合溶剂中反应,得到含ＭｏＦｅ_３Ｓｅ_４核芯的Ｍｏ－Ｆｅ－Ｓｅ簇合物ＭｏＦｅ_３Ｓｅ_４（μ－Ｒ_２ＮＣＳ_２）_２（Ｒ_２ＮＣＳ_２）_４（Ｒ２＝Ｍｅ_２（１）,Ｅｔ_２（２）,Ｃ_４Ｈ_８（３））．化合物２的单晶Ｘ射线衍射分析表明,其分子结构为２个桥式和４个螫合Ｅｔ_２ＮＣＳ_２~－配体包围的一个扭曲类立方烷Ｍ_４Ｓｅ_４簇核对３个化合物的ＣＶ进行了表征,它们在ＤＭＳＯ溶液中的电化学行为表现出了多电子可逆的传递过程．     

6-硫杂-13-氧杂二环[9.3.0]-3,8-二炔十四烷的合成及核磁共振鉴定

以３，４－二（４′－甲磺酰氧－２′－丁炔基）四氢呋喃或６－硫杂－３，８－二炔－１，１１－二羟甲基环十一烷为原料合成了二环化合物６－硫杂－１３－氧杂二环［９．３．０］－３，８－二炔十四烷。通过１ＨＮＭＲ，１３ＣＮＭＲ，ＩＲ及ＭＳ进行了结构鉴定。     

稠杂环化合物的研究（XV）──6－取代－3－（1H－苯并三唑－1－亚甲基）－1，2，4－三唑并［3，4－b］－1，3，4－噻二唑的合成

研究了３－（１Ｈ－苯并三唑－１－亚甲基）－４－氨基－５－巯基－１，２，４－三唑与取代苯甲酸在三氯氧磷催化下的反应，制得１０种新的３－（１Ｈ－苯并三唑－１－亚甲基）－１，２，４．三唑并［３，４－ｂ］－１，３，４－噻二唑，通过元素分析、ＩＲ、￣１ＮＭＲ和ＭＳ确证了它们的结构并讨论了其波谱性质。     

Synthesis of 3H-labeled Efomycine M

For in-depth characterization as a putative pan-selectin antagonist 3H-labeled Efomycine M was synthesized starting from the natural product derived from Elaiophyline.     

用偶氮胂M分光光度法测定蛋白质

研究了蛋白质与偶氮胂 M的显色反应。在含 0 .0 5 0 % OP的 p H2 .5的缓冲溶液中 ,偶氮胂 M与蛋白质形成兰色复合物 ,λmax为 60 5 nm,ε为 4.5× 1 0 5L· mol- 1· cm- 1,蛋白质含量在 3.3～ 2 5 4 mg/L范围内 ,服从比耳定律。所提出的方法可直接用于血清、花生等生物样品中蛋白质含量测定     

Studies on HEPES Stabilizing M Intermediate of Bacteriorhodopsin

ＳｔｕｄｉｅｓｏｎＨＥＰＥＳＳｔａｂｉｌｉｚｉｎｇＭＩｎｔｅｒｍｅｄｉａｔｅｏｆＢａｃｔｅｒｉｏｒｈｏｄｏｐｓｉｎＦＵＸｕｅ－ｑｉ￣１,ＬＩＺｈｅｎｇ－ｑｉａｎｇ￣２,ＷＡＮＧＪｉｎ－ｄｕｉ￣１,ＷＡＮＧＢａＯ－ｈｕｉａ,ＬＩＢｏ－ｆｕ￣２ａｎｄＬＩ...     

钛,锆和铪羰基化合物M(CO)_n(M=Ti,Zr,Hf;n=4～7)的理论研究

利用密度泛函方法对标题化合物的平衡几何、热化学及振动频率进行了理论预测,发现这3种金属原子都有相似的M(CO)n(n=4～7)结构.全局最低构型对M(CO)7都是单态C3v戴帽八面体7S-1,对M(CO)6都是三重态D3d畸变八面体6T(而对应的单重态M(CO)5仅比它低不到21 kJ·mol-1).对M(CO)n(n=5,4)都是三重态6S-1,其构型分别为从6T中移去1个或2个CO基的衍生物5T和4T.此外,五重态的D3h的三角双锥M(CO)5和单态的Td四面体M(CO)4以及能量更高的含有C和O同时与金属成键的独特配位CO基的M(CO)6和M(CO)3也被发现.最后,给出M(CO)7→M(CO)6+CO反应的离解能.并讨论了金属18价电子的Ti(CO)7存在的可能性.     

TG(M) and DTG(M) Techniques and Some of Their Applications on Material Study

Adding a magnetic field gradient to the conventional TG system constructs the magnetic thermogravimetry analysis (TG(M) i.e. Faraday methods) and the magnetic derivative thermogravimetry (DTG(M)) techniques. We used the techniques to study the nanocrystalline processes of the FeCuNbSiB and FeCuNbCoSiB amorphous alloys. Some problems of their applications such as the characteristic temperature T_min and T_C are also discussed in detail.This revised version was published online in November 2005 with corrections to the Cover Date.     

选择性M3受体拮抗剂的研究进展

M3受体是毒蕈碱型乙酰胆碱受体的亚型之一,在人体内分布广泛。选择性M3受体拮抗剂可以竞争性地与M3受体结合,主要用于膀胱过度活动症(OAB)、慢性阻塞性肺病(COPD)和肠道易激综合症(IBS)等疾病的治疗。与非选择性拮抗剂相比,选择性M3受体拮抗剂对中枢神经以及心脏的副作用大大降低。本文对已上市及处在不同研究阶段的选择性M3受体拮抗剂进行了综述。     

Antigen targeting to M cells for enhancing the efficacy of mucosal vaccines

Vaccination is one of the most successful applications of immunology and for a long time has depended on parenteral administration protocols. However, recent studies have pointed to the promise of mucosal vaccination because of its ease, economy and efficiency in inducing an immune response not only systemically, but also in the mucosal compartment where many pathogenic infections are initiated. However, successful mucosal vaccination requires the help of an adjuvant for the efficient delivery of vaccine material into the mucosa and the breaking of the tolerogenic environment, especially in oral mucosal immunization. Given that M cells are the main gateway to take up luminal antigens and initiate antigen-specific immune responses, understanding the role and characteristics of M cells is crucial for the development of successful mucosal vaccines. Especially, particular interest has been focused on the regulation of the tolerogenic mucosal microenvironment and the introduction of the luminal antigen into the lymphoid organ by exploiting the molecules of M cells. Here, we review the characteristics of M cells and the immune regulatory factors in mucosa that can be exploited for mucosal vaccine delivery and mucosal immune regulation.     

Spectrophotometric Study on the Interaction between Arsenazo M and Proteins

Dye binding protein assays are commonly used in biochemical and clinical laboratories, and the reaction mechanism is still under investigation1-2. In this paper, the interaction of Arsenazo M with serum proteins was studied. Procedure In most experiments, 1.20 mL of Arsenazo M (5.0010-4 mol/L), 2.0 mL of C-L buffer solution, 3.0 mL alcohol and certain amount of protein standard solutions or samples were added to 10 mL volumetric flasks, then diluted to mark with water, and mixed thor…     

Molecular Recognition of Aflatoxin M1 in Water and Milk Samples

Two stochastic microsensors based on diamond paste modified with 2,2‐diphenyl‐1‐picrylhydrazyl (DPPH) were proposed for the molecular recognition of aflatoxin M1 in water and milk samples. Two types of diamond were used: a monocrystalline diamond powder (1 μm) (DP) and a nanopowder of monocrystalline diamond (10 nm) (nDP) for the design of the stochastic microsensors. The microsensors were incorporated as combined stochastic microsensors (a microcell containing the stochastic microsensor and the Pt wire, and a Ag/AgCl sensor) in a platform used for monitoring of waste waters and milk samples. The platforms were used for the fast screening of water and milk samples for the qualitative and quantitative analysis of aflatoxin M1 at very low concentration levels (up to 0.001 fg/L). The linear concentration ranges were wide, being able to cover concentrations between 0.001 fg/L to 20 μg/L. The highest sensitive microsensor (sensitivity of 4.74×10¹⁰ s mg^?1 L) was the one based on nDP. The results provided by the platforms were in agreement with those obtained by utilization of standard method (ISO certified methods (HPLC/fluorescence method)), recoveries being higher than 99.00 % and RSD lower than 1.00 % proving that the method can be reliable used for molecular recognition of aflatoxin M1 in water and milk samples.     

免疫纳米金催化共振散射光谱法测定痕量IgM

用粒径为10 nm的金纳米微粒标记羊抗人免疫球蛋白M（IgM）,制备了IgM的免疫纳米金共振散射光谱探针。在pH4.49的KH2PO4-Na2HPO4缓冲溶液及PEG存在下,金标羊抗人IgM与IgM发生特异性结合生成胶体金免疫复合物,离心分离,获得未反应的金标抗上层清液。以此纳米金标抗作为催化剂,在pH 1.93的盐酸-柠檬酸钠缓冲溶液,催化NH2OH·HCl还原吸附在免疫纳米金表面的金络离子物种（AuCl4-）生成粒径更大的金纳米微粒,导致580 nm 处金纳米微粒的共振散射强度急剧增大。结果表明,随着IgM浓度增大,离心上层液中金标抗降低,I 580 nm线性降低,其△I580 nm与IgM浓度在0.06～4.80 ng· ml-1范围内呈良好的线性关系,其回归方程为ΔI580 nm=14.5cIgM + 1.8,检出限为0.03 ng·ml-1。本法具有灵敏、快速和较高的特异性,用于定量分析人血清中IgM,结果满意。