高效液相色谱—化学发光法研究异烟肼和利福平

基于异烟肼和利福平在碱性介质中能与K3Fe(CN)6反应产生强的化学发光，因 此设计了一个经高效液相色谱（HPLC）分离柱后同时检测一线抗结构病药物异烟肼 、利福平的化学发光检测器。研究并优化了流动相、流速以及化学发光检测的条件 。该方法测定异烟肼、利福平的线性范围分别为0.05～6.0mg/L，0.08～20.0mg/L ，其检出限：异烟肼为2×10^-2mg/L，利福平为4×10^-2mg/L，测定的相对标准偏 差分别为1.9，2.9。该方法已成功地用于同时测定复方利福平片中利福平和异烟肼 的含量。     

Synthesis and Properties of Novel Hemicyanine Dye-β-Cyclodextrin

A series of novel hemicyanine dye-β-cyclodextrin compounds： mono-6-deoxy-β-cyclodextrin-6-[p-（p-substituted styryl）pyridium] p-totylfulfonates were synthesized by the condensation of mono-6-deoxy-β- cyclodextrin-6-（p-methyl pyridinium） p-toluenesulfonate with （un）substituted benzaldehydes. Their structures were established by 1^H NMR, IR, UV-Vis and elemental analysis. The absorption and fluorescence properties of the novel compounds were measured in solution and the photostability of a selected hemicyanine dye-β-cyclodextrin compound was also investigated.     

Energy Transfer Electrogenerated Chemiluminescence for the Determination of Sulfite

A simple and novel electrogenerated chemiluminescence (ECL) method for the determination of sulfite has been developed based on the energy transfer ECL process. It was found that a weak ECL signal of sulfite was electrochemically generated on a platinum electrode in neutral aqueous solution. The signal was strongly enhanced by rhodamine B as an energy receptor and further enhanced by the neutral surfactant Tween 80. In 0.10M phosphate buffer solution (pH=7.5) containing 2.0×10^–6gmL^–1 rhodamine B and 0.4% (v/v) Tween 80, the ECL response to the concentration of sulfite at a potential of 0.82V was linear over a range of 1.0×10^–7gmL^–1 to 8.0×10^–6gmL^–1, and the detection limit was 5×10^–8gmL^–1. The relative standard deviation (n=11, 1.0×10^–6gmL^–1) was 3.8%. The proposed method has been successfully applied to the determination of sulfite in pharmaceutical injections and white sugar samples.     

Chemistry of borate in salt lake brine (XXXIV)

The crystallization processes of hydrated Mg-borates, boric, magnesium hydroxide and Mg-oxychloride from MgO-B₂O₃-18%MgCl₂-H₂O supersaturated solution at 20°C have been studied by kinetic method. The crystallization solid phases were characterized by X-ray powder diffraction, IR spectra, thermal analysis and chemical analysis. The liquid-solid phase diagram of thermodynamic nonequilibrium state has been given. In this phase diagram, there exist eight crystallization fields, boric acid(H₃BO₃), trigomagneborite(MgO · 3B₂O₃ · 7.5H₂O, MgO · 3B₂O₃ · 7H₂O), hungchaoite(MgO · 2B₂O₃ · 9H₂O), inderite(2MgO · 3B₂O₃ · 15H₂O), chloropinnoite(2MgO · 2B₂O₃ · MgCl₂ · 14H₂O), magnesium hydroxide(Mg(OH)₂) and magnesium oxychloride (5Mg(OH)₂ · MgCl₂ · 8H₂O).     

高中有机化学教材“烃类化合物”的国际比较研究

基于闫春更等建立的二维度四指标教材难度微观评价模型，重点对中国、美国、新加坡、澳大利亚、日本、英国的高中化学教材中"烃类化合物"内容的整合广度、表征深度进行测评和比较。研究发现6国教材内容的整合广度整体上差异不大，但其表征深度差异明显；美国教材注重学生认识物质的思路和方法的渗透，日本教材注重基本知识与技能的掌握，中国教材将概念诠释与样例分析相融合；英国、新加坡、美国教材注重情境推理或比较等信息处理策略的运用，对学习者学习的引导性较强。     

Synthesis and Crystal Structure of [Co(H<Subscript>2</Subscript>O)<Subscript>6</Subscript>](C<Subscript>19</Subscript>H<Subscript>17</Subscript>O<Subscript>4</Subscript>SO<Subscript>3</Subscript>)<Subscript>2</Subscript>⋅8H<Subscript>2</Subscript>O

The title compound, cobalt 4′,7-diethoxylisoflavone-3′-sulfonate([Co(H₂O)₆](X)₂⋅8H₂O, X = C₁₉H₁₇O₄SO₃) was synthesized and its structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in the triclinic space group P-1 with cell parameters a = 9.026(3) Å, b = 16.431(5) Å, c = 18.195(6) Å, α = 72.289(4)^∘, β = 87.498(4)^∘, γ = 82.775(5)^∘, V = 2550.1(13) Å⁻³, D_c = 1.419 Mg m⁻³, and Z = 2. The results show that the title compound consists of one cobalt cation, six coordinated water molecules, eight lattice water molecules, and two 4′,7-diethoxylisoflavone-3′-sulfonate anions, C₁₉H₁₇O₄SO⁻₃. Two anions have different conformations. Twelve H atoms of six coordinated water molecules, as donors, form hydrogen bonds with four oxygen atoms of sulfo-groups of two anions and eight oxygen atoms of eight lattice water molecules. In addition, π < eqid1 > ⋅ < eqid2 > π stacking interactions exist in the crystal structure, which together with hydrogen bonds lead to supramolecular formation with a three-dimensional network.     

2-Oxo-3,4-dihydropyrimido[4,5-d] pyrimidines as new reversible inhibitors of EGFR C797S (Cys797 to Ser797) mutant

Extensive structure-activity relationships (SARs) study of JND3229 was conducted to yield a series of new reversible 2-oxo-3,4-dihydropyrimido[4,5-d]pyrimidine privileged scaffold as EGFR^C797S inhibitors. One of the most potent compound 6i potently suppressed EGFR^{L858R/T790M/C797S} kinase with an IC₅₀ value of 3.1 nmol/L, and inhibited the proliferation of BaF3 cells harboring EGFR^{L858R/T790M/C797S} and EGFR^{19D/T790M/C797S} mutants with IC₅₀ values of 290 nmol/L and 316 nmol/L, respectively. Further, 6i dose-dependently induced suppression of the phosphorylation of EGFR^{L858R/T790M/C797S} and EGFR^{19D/T790M/C797S} in BaF3 cells. Compound 6i may serve as a promising lead compound for further drug discovery overcoming the acquired resistance of non-small cell lung cancer (NSCLC) patients.     

Radiometric analysis of Chinese commercial granites

Summary Due to the widespread use of granites as building and ornamental materials, measurements of ²²⁶Ra, ²³²Th and ⁴⁰K activities in commercial granites have been carried out using a NaI(Tl)g-ray spectrometer with a matrix-inversion-based spectral stripping technique. The concentrations of ²²⁶Ra, ²³²Th and ⁴⁰K in Chinese commercial granite range from 14.5 to 204.7 Bq^. kg^-1, 16.7 to 186.7 Bq^. kg^-1and 185.7 to 1745.6 Bq^. kg^-1, respectively. The mean values of the activity concentrations of ²²⁶Ra, ²³²Th and ⁴⁰K in red and pink commercial granites are all higher than those in black and gray commercial ones. The radium equivalent activity (Ra_eq), the external hazard index (H_ex), the internal hazard index (H_in ) and the annual gonadal dose equivalent (AGDE) were also calculated and compared to the international recommended values. Six types of red commercial granites (CBR, MLR, QXR, PBR, JXR, LQR, YDR and TSR) of China do not satisfy the universal standards.     

Hydroxylamine derivative in the Purex Process

N,Ndiethylhydroxylamine (DEHAN) can rapidly reduce Pu(IV) and Np(VI) extractable with trinbutyl phosphate (TBP) to Pu(III) and Np(V) unextractable with TBP in nitric acid solution. In order to apply DEHAN in the purification cycle step of U (noted as contactor 2D) of the secondcycle of the Purex Process to separate Np and Pu from U, the reduction of Np(VI) and the stability of Np(V) with DEHAN and the singlestage reduction extraction and backextraction of Np(VI) have been studied according to the experimental conditions of contactor 2D. The results show that more than 99% of Np(VI) can entirely be reduced to Np(V) with DEHAN within a few minutes either in aqueous or in organic phase containing uranium and without containing uranium, and more than 99% of Np(VI) can be backextracted from the organic to the aqueous phase with DEHAN as a reductant. More than 99% of Np(V) exists in nitric acid solution at least for 8 hours in presence of 0.01 mol/l DEHAN. These results are of benefit to the cascade extractionseparation of U/Np in contactor 2D in order to decontaminate Np from U.     

Hydroxylamine Derivative in Purex Process III. The Kinetics of Oxidation-reduction Reaction Between N,N-diethylhydroxylamine and Neptunium(VI)

The kinetics of oxidation-reduction reaction between N,N-diethylhydroxylamine (DEHAN) and neptunium (VI) in nitric acid media has been studied by spectrophotometry at 25.2 °C. The rate equation is -d[Np(VI)/dt=k[Np(VI)][DEHAN]/[H⁺] found by investigating the influence of concentration, acidity, ionic strength and temperature on the reaction. The rate constant of the reaction k is 23.0±1.8 min^–1 for = 2.0 mol/l. A possible mechanism of reaction has been suggested according to the ESR spectra of nitroxide radical produced in the DEHAN+V(V) system.