合成香料β-大马酮的高效液相色谱分析

本文提出了用分析型HPLC仪器制备β-大马酮标准品的方法及用HPLC测定β-大马酮含量的方法。制备色谱柱为Zorbax SIL 9.4 mmφ×25cm,流动相为石油醚(30～60℃)/乙醚98.5/1.5。分析用色谱柱为Shim CLC SIL 6 mmφ×15cm(岛津全多孔硅胶柱),流动相为石油醚(60—90℃)/无水乙醇99.88/0.12,检测器为紫外可见分光光度检测器。波长253nm或302nm,标准曲线的线性范围0～1.4mg/ml。峰高或峰面积均可用于测定,回收率100.7%。     

羧甲基壳聚糖对胆红素的吸附性能研究

合成了不同取代度的羧甲基壳聚糖(CM-CTS)作为吸附剂，研究了不同条件对CM-CTS吸附胆红素性能的影响．结果表明：在实验条件下，随着羧甲基取代度的增加和体系温度的升高．最大吸附率和吸附速率均相应增加：在接近人体血液pH值的条件下，CM-CTS对胆红素的吸附性能较佳：人血清白蛋白和离子强度的增加对CM—CTS吸附胆红素有明显的抑制作用。     

Applications of column-switching technique in biopharmaceutical analysis. I. High-performance liquid chromatographic determination of amitriptyline and its metabolites in human plasma

A new high-performance liquid chromatographic method for the determination of amitriptyline and its metabolites, nortriptyline, 10-hydroxynortriptyline and 10-hydroxyamitriptyline, in plasma is described which uses direct injection and a column-switching valve. The method is based on the enrichment of drugs on a reversed-phase concentration column, packed with Corasil RP. The enriched drugs were then separated, using back-flush mode on a bonded-phase CN column using an isocratic acetonitrile-acetate buffer (60:40, v/v) mobile phase. The validation of the method showed excellent sensitivity, precision and reproducibility. The limit of detection, using a 250-microliter direct injection of plasma, was between 5 and 10 ng/ml for each of the four drugs. The mean coefficient of variation for intra- and inter-assay was better than 5%. The method showed obvious advantages over conventional extraction procedures in terms of speed and ease of sample handling. The method has been successfully applied to the samples from patients receiving oral doses of amitriptyline.     

Mössbauer study of the three-coordinate planar Fe(II) thiolate complex [Fe(SR)(3)](-) (R = C(6)H(2)-2,4,6-tBu(3)): model for the trigonal iron sites of the MoFe(7)S(9):homocitrate cofactor of nitrogenase

The cofactor (M-center) of the MoFe protein of nitrogenase, a MoFe(7)S(9):homocitrate cluster, contains six Fe sites with a (distorted) trigonal sulfido coordination. These sites exhibit unusually small quadrupole splittings, Delta E(Q) approximately 0.7 mm/s, and isomer shifts, delta approximately 0.41 mm/s. M?ssbauer and ENDOR studies have provided the magnetic hyperfine tensors of all iron sites in the S = 3/2 state M(N). To assess the intrinsic zero-field splittings and hyperfine parameters of the cofactor sites, we have studied with M?ssbauer spectroscopy two salts of the three-coordinated Fe(II) thiolate complex [Fe(SR)(3)](-) (R = C(6)H(2)-2,4,6-tBu(3)). One of the salts, [Ph(4)P][Fe(SR)(3)] x 2MeCN x C(7)H(8), 1, has a planar geometry with idealized C(3h) symmetry. This S = 2 complex has an axial zero-field splitting with D = +10.2 cm(-1). The magnetic hyperfine tensor components A(x) = A(y) = -7.5 MHz and A(z) = -29.5 MHz reflect an orbital ground state with d(z(2)) symmetry. A(iso) = (A(x) +A(y) +A(z))/3 = -14.9 MHz, which includes the contact interaction (kappa P = -21.9 MHz) and an orbital contribution (+7 MHz), which is substantially smaller than A(iso) approximately -22 MHz of the tetrahedral Fe(II)(S-R)(4) sites of both rubredoxin and [PPh(4)](2)[Fe(II)(SPh)(4)]. The largest component of the electric field gradient (EFG) tensor is negative, as expected for a d(z(2)) orbital. However, Delta E(Q) = -0.83 mm/s, which is smaller than expected for a high-spin ferrous site. This reduction can be attributed to a ligand contribution, which in planar complexes provides a large positive EFG component perpendicular to the ligand plane. The isomer shift of 1, delta = 0.56 mm/s, approaches the delta-values reported for the six trigonal cofactor sites. The parameters of 1 and their importance for the cofactor cluster of nitrogenase are discussed.     

羧甲基壳聚糖/聚乙烯醇/甘油环氧树脂蛇笼型复合螯合膜的制备及对金属离子的吸附性能

以交联甘油环氧树脂交联的聚乙烯醇(PVA)为笼树脂，羧甲基壳聚糖(CCTS)为蛇树脂制备了具有蛇笼结构的复合螯合膜，研究了其对Cu^2 、Ni^2 、Pb^2 、Fe^3 、Zn^2 ，Hg”^2 、Cd^2 等金属离子的吸附性能，研究表明，该树脂对Cu^2 、Ni^2 、Pb^2 有较好的吸附性能，其中PVA是对Cu^2 的吸附的主要贡献者，而CCTS则是在对Ni^2 的吸附中起主要作用。该树脂可以用于含Cu^2 废水的处理。     

A RELATION BETWEEN THE APPARENT VELOCITY AND THE SPECTRAL POWER OF SUPERLUMINAL RADIO SOURCES

It is proved that the apparent transverse velocities β_(app) and the spectral powers at 10GHz P_(10) of the cores of known superluminal sources are correlated. An interpretation ofthis result within the framework of the relativistic jet model shows that the jet Lorentzfactor γ depends on the intrinsic luminosity of the sources. The probable existence of twosubpopulations of the superluminal sources is shown by a linear regression analysis. "Small"sources f i.e. the sources without extended emission or with a distance from the core tothe outer edge of the lobe<20 kpc, show lower β_(app) than the "large" objects; this can beinterpreted as an orientation effect. Since all BL Lac objects belong to the "small" class,this result sheds new light on such a question as why these sources have lower apparent ve-locities than the "classical" superluminal quasars.     

Gallium-boron donor-acceptor bonds

Examples of compounds with gallium-boron donor-acceptor bonds, HC[MeC(2,6-pri2C6H3)N]2Ga-->B(C6F5)3 3 and (eta 5-C5Me5)Ga-->B(C6F5)3 4 have been prepared by treatment of the free gallanediyls with B(C6F5)3; the structures of both compounds were determined by X-ray crystallography.     

β-榄香烯振动光谱的量子化学从头计算

利用G98及GAMESS从头计算程序的RHF／6－31方法,对β－榄香烯的全部振动基频作了计算,并与实测红外光谱做了对比,归属了它们的振动模式,讨论了它们的特征基频,并对理论计算的振动频率进行了标度校正。     

Hierarchical nanostructured composite cathode with carbon nanotubes as conductive scaffold for lithium-sulfur batteries

Carbon nanotubes (CNTs) are excellent scaffolds for advanced electrode materials, resulting from their intrinsic sp2 carbon hybridization, interconnected electron pathway, large aspect ratio, hierarchical porous structures, and low cost at a large-scale production. How to make full utilization of the mass produced CNTs as building blocks for nanocomposite electrodes is not well understood yet. Herein, a composite cathode containing commercial agglomerated multi-walled CNTs and S for Li-S battery was fabricated by a facile melt-diffusion strategy. The hierarchical CNT@S coaxial nanocables exhibited a discharging capacity of 1020 and 740 mAh g-1 at 0.5 and 2.0 C, respectively. A rapid capacity decay of 0.7% per cycle at the initial 10 cycles and a slow decay rate of 0.14% per cycle for the later 140 cycles were detected. Such hierarchical agglomerated CNT@S cathodes show advantages in easy fabrication, environmentally benign, low cost, excellent scalability, and good Li ion storage performance, which are extraordinary composites for high performance Li-S battery.     

Coral reef-like polyanaline nanotubes prepared by a reactive template of manganese oxide for supercapacitor electrode

Coral reef-like PANI nanotubes composed of nanopaticles were successfully synthesized by a reactive template of manganese oxide.The structure was characterized by using SEM,TEM,and FT-IR,and the supercapacitive behaviors of these nanotubes were investigated with cyclic voltammetry（CV）,and charge-discharge tests,respectively.A maximum specific capacitance of 533 F/g could be achieved in 1mol/L aqueous H₂SO₄ with the potential range of -0.2 to 0.8 V（vs.the saturated calomel electrode） in a half-cell setup configuration for PANI electrode,suggesting its potential application in the electrode material for electrochemical capacitors.