HPLC测定怀菊花中的总黄酮

建立了HPLC测定怀菊花中总黄酮含量的方法.采用Agilent C18柱(150mm×4.6mm,5μm),以甲醇(A)-超纯水(0.2％的冰乙酸)(B)(25∶75,V/V)为流动相,流速:0.5mL·min-1;柱温为20℃,检测波长:260nm;进样量:10μL.结果:回归方程为y=33.29x-8.284,r=0.9993(n=6),线性范围0-20μg,平均回收率为102.63％,RSD为5.56％.样品总黄酮含量为7.51mg/g.方法简便、灵敏、快速、准确、重现性好,可用于怀菊花中总黄酮含量的质量控制.     

Change in the particle size of highly dispersed palladium black in hydrochloric acid solutions at elevated temperatures

The growth of palladium black at 130 and 180°C was studied in detail using transmission electron microscopy and X-ray diffraction. It was found that the solution of palladium metal due to the presence of chemisorbed oxygen occurred in hydrochloric acid solutions. A procedure was proposed for the removal of oxygen from the surface of palladium black without noticeable changes in its structural characteristics.     

Indirect method for determining silicon and phosphorus, and analysis of cuban laterites

A method has been developed for determining silicon and phosphorus in minerals with high iron content, the method being based on the formation, extraction and stripping of molybdenum heteropoly acids and determination of molybdenum after decomposition of the complexes in the aqueous phase from the stripping.     

High temperature solid state catalytic isotope exchange with deuterium and tritium

A method for synthesizing tritium- or deuterium-labeled amino acids, peptides and biogenic amines through high temperature solid state catalytic isotope exchange (HSCIE) is proposed. The dependence of the degree of isotope exchange in HSCIE on the structure of the compound, the reactivity of hydrogen at different carbon atoms and the conditions of the process has been examined. If HSCIE is performed in the temperature range of 373 to 413K, the selectivity of isotopic label incorporation comes to 70% or higher. When the tritium label is introduced into peptides, they retain the configuration of asymmetric atoms, even upon the substitution of tritium for hydrogen at the -carbon atoms of the amino acid residues. HSCIE at 453–513K leads to an even distribution of the isotopic label over the organic compound molecule. The results of³H NMR spectroscopy highlighting the distribution of the tritium label in the organic compound molecules are presented. The configuration of asymmetric atoms in amino acids is preserved to a high extent upon 80–90% substitution of isotopes for hydrogen atoms.Presented at the 12th Radiochemical Conference, Marianské Lazné May 7–11, 1990.     

Synthesis and structure of zirconium and 3d-transition metal phosphates M 0.5Zr2(PO4)3(M = Mn, Co, Ni, Cu, Zn)

Double zirconium and 3d-transition metal phosphates of the compositions M 0.5Zr2(PO4)3[M = Mn (I), Co (II), Ni (III), Cu (IV), Zn (V)] have been synthesized and the types of their structures have been refined. Compounds I, II, III, IV, and V are all monoclinic (sp. gr. P2₁/n, Z = 4) and have the unit cell parameters a = 12.390(3), 12.389(3), 12.385(3), 12.389(3), 12.389(2) Å; b = 8.931(4), 8.928(3), 8.924(4), 8.925(4), 8.929(3) Å; c = 8.843(3), 8.840(2), 8.840(3), 8.841(3), 8.842(2) Å, β = 90.55(1), 90.54(1), 90.53(1), 90.53(1), 90.54(1)°; V = 978.5, 977.7, 977.0, 977.4, 978.1 ų, respectively. All the structures have the {[Zr₂(PO₄)₃]^?}3_∞-type frameworks. The crystallographic data for 3d-transition and alkali earth metal phosphates described by the general formula M _0.5Zr₂(PO₄)₃ are compared.     

非有机溶剂液-固萃取体系提取血红蛋白研究

用聚乙二醇(PEG8000)修饰物混合吐温80-磷酸钾盐液-固萃取体系从血液中直接提取血红蛋白,考察了PEG8000修饰物、磷酸钾盐和吐温80的浓度及酸度和温度等因素对血红蛋白分离纯化的影响.结果表明,采用该体系的一次固相萃取率大于99%,一次反萃取率达到75%.所得到的血红蛋白干粉的纯度为99%.该方法不使用有机溶剂,无毒性,对蛋白质具有稳定和保护作用,易于放大规模使用.     

Architecture of phosphates with {[L 2(PO4)3] p−}3∞ frameworks

The general principles of the structural organization for the existing types of orthophosphates with the {[L ₂(PO₄)₃] ^p?}_3∞ frameworks, where L is an octahedrally coordinated ion, are discussed. Representing these frameworks by double LP₆-octahedra, it is possible to find out the related structures and analyze their symmetry relation.     

勾形磁场对分离结晶法制备CdZnTe晶体的影响

为了了解勾形磁场对CdZnTe晶体生长质量的影响,利用有限元法对坩埚内的热量和动量传递过程进行了全局数值模拟。假定熔体和气相中的流动都为准稳态轴对称层流,研究了B_o(磁场轴线与晶体-坩埚界面的交点的磁场强度的轴向分量)为0 T,0.5 T,1.0 T,1.5 T,2.0 T,2.5 T,3.0 T时的CdZnTe晶体生长过程。结果表明:勾形磁场能有效抑制熔体内的流动,会产生由洛仑兹力、表面张力和浮力共同驱动的涡胞。随着磁场强度的增加,传热向导热型转变,熔体内最大流函数逐渐减小,抑制作用增强。     

Reversible dissociation of dibromobromates in organic solvents

A study was carried out on the reversible decomposition of dibromobromate anions in organic solvents and we found the equilibrium constants for the processes responsible for the distribution of active halogen and hydrogen halide between their different forms in solution. The capacity of the solvent to form hydrogen bonds with the bromide anion, the feasibility of forming a molecular complex with bromine, and the structure of the cation (in solutions with low ionizing capacity) were all found to affect the reversible decomposition of the dibromobromate anion. Translated from Teoreticheskaya i éksperimental'naya Khimiya, Vol. 44, No. 5, pp. 298–305, September–October, 2008.