湿热证动物模型微量元素、维生素E变化及清香散的调节作用

采用多因素造模方法复制成湿热证动物模型，观察了动物模型微量元素Zn、Cu、Fe、Se和维生素E代谢水平的变化。结果显示，模型动物血清Zn下降（P＜0．05），Cu升高（P＜0．05或P＜0．01），Fe变化不大（P＞0．05），血Se水平下降（P＜0．05），血浆维生素E含量减少（P＜0．01）。经清热祛湿的经验方清香散治疗后，治疗I组动物血清Zn、血Se、血浆维生素E明显升高（P＜0．05），血清Cu下降（P＜0．05）；治疗Ⅱ组血浆血清Cu有变化（P＜0．05）外，其余变化不大。     

微波辅助快速制备2D/1D ZnIn2S4/TiO2 S型异质结及其光催化制氢性能

The threat and global concern of energy crises have significantly increased over the last two decades. Because solar light and water are abundant on earth, photocatalytic hydrogen evolution through water splitting has been considered as a promising route to produce green energy. Therefore, semiconductor photocatalysts play a key role in transforming sunlight and water to hydrogen energy. To date, various photocatalysts have been studied. Among them, TiO₂ has been extensively investigated because of its non-toxicity, high chemical stability, controllable morphology, and high photocatalytic activity. In particular, 1D TiO₂ nanofibers (NFs) have attracted increasing attention as effective photocatalysts because of their unique 1D electron transfer pathway, high adsorption capacity, and high photoinduced electron–hole pair transfer capability. However, TiO₂ NFs are considered as an inefficient photocatalyst for the hydrogen evolution reaction (HER) because of their disadvantages such as a large band gap (~3.2 eV) and fast recombination of photoinduced electron–hole pairs. Therefore, the development of a high-performance TiO₂ NF photocatalyst is required for efficient solar light conversion. In recent years, several strategies have been explored to improve the photocatalytic activity of TiO₂ NFs, including coupling with narrow-bandgap semiconductors (such as ZnIn₂S₄). Recently, microwave (MW)-assisted synthesis has been considered as an important strategy for the preparation of photocatalyst semiconductors because of its low cost, environment-friendliness, simplicity, and high reaction rate. Herein, to overcome the above-mentioned limiting properties of TiO₂ NFs, we report a 2D/1D ZnIn₂S₄/TiO₂ S-scheme heterojunction synthesized through a microwave (MW)-assisted process. Herein, the 2D/1D ZnIn₂S₄/TiO₂ S-scheme heterojunction was constructed rapidly by using in situ 2D ZnIn₂S₄nanosheets decorated on 1D TiO₂ NFs. The loading of ZnIn₂S₄ nanoplates on the TiO₂ NFs could be easily controlled by adjusting the molar ratios of ZnIn₂S₄ precursors to TiO₂ NFs. The photocatalytic activity of the as-prepared samples for water splitting under simulated solar light irradiation was assessed. The experimental results showed that the photocatalytic performance of the ZnIn₂S₄/TiO₂ composites was significantly improved, and the obtained ZnIn₂S₄/TiO₂ composites showed increased optical absorption. Under optimal conditions, the highest HER rate of the ZT-0.5 (molar ratio of ZnIn₂S₄/TiO₂= 0.5) sample was 8774 μmol·g^-1·h^-1, which is considerably higher than those of pure TiO₂ NFs (3312 μmol·g^-1·h^-1) and ZnIn₂S₄nanoplates (3114 μmol·g^-1·h^-1) by factors of 2.7 and 2.8, respectively. Based on the experimental data and Mott-Schottky analysis, a possible mechanism for the formation of the S-scheme heterojunction between ZnIn₂S₄ and TiO₂ was proposed to interpret the enhanced HER activity of the ZnIn₂S₄/TiO₂heterojunctionphotocatalysts.      

高效毛细管电泳电导法快速检测复方维生素B片中的VB1、VB12、VB6和VC

采用高效毛细管电泳电导法同时分离、测定了复方维生素B片中的主要成分VB1, VB12,VB6和VC的含量.研究了运行缓冲溶液的酸度和浓度、电泳电压、进样时间等因素对电泳的影响.在优化的实验条件下40 mmol/L Tris -4 mmol/L H3BO3 (pH 8.0) 的缓冲溶液中加入0.30 mmol/L CTAB(溴化十六烷基三甲基铵),分离电压为15 kV,上述4组分在5 min内得到良好的分离.维生素B1,B12,B6和VC的线性范围分别为5.5～1.0 mg/mL; 15～1.5 mg/mL; 1.0～0.40 mg/mL和6.6～0.80 mg/mL; 检测限分别为0.80 μg/mL, 4.0 μg/mL, 0.50 μg/mL, 2.9 μg/mL; 5次测定峰高的相对标准偏差分别为2.2%, 1.6%, 3.9%, 2.8%.5次测定的平均回收率分别为99%, 94%, 100%, 97%.     

D,L-1,2,2-三甲基环戊烷-1,3-二胺硝酸镍配合物的合成、结构及其和手性D-(+)-1,2,2-三甲基环戊烷-1,3-二胺氯化镍配合物的对比分析(英)

A nickel(Ⅱ) complex [Ni(La)₂](NO₃)₂ (1) with bidentate racemic 1,2,2-trimethylcyclopentane-1,3-diamine ligand has been synthesized and characterized by IR, EA, ES-MS, and its X-ray diffraction study reveals that the nickel(Ⅱ) center is tetra-coordinated by one D- and one L- diamine ligands, and a three-dimensional hydrogen-bond-sustained network is formed in the solid state by means of the eight-membered N-H…O hydrogen bond cycle. This compound also supplies a good comparison to the chiral complex [Ni(L_b)₂]Cl₂·2H₂O (2) (L_b=D-(+)-1,2,2-trimethylcyclopentane-1,3-diamine). CCDC: 218122.     

缝管原子捕集原子吸收光谱法测定维生素B12

本文研究了Ａｌ２Ｏ２涂层的开缝石英管原子捕集法测定ＣＯ的条件并通过测ＣＯ间接测定维生素Ｂ（１２）。结果表明，在优化条件下Ｃｏ的特征浓度为８×１０（－３）μｇ·ｍＬ（－１），比常规火焰原子吸收法的灵敏度提高８倍。采用本法测定腺苷辅酶维生素Ｂ（１２）中ＶＢ（１２）的含量，相对标准偏差１．１％，加标回收率９８．２～１００．４％。     

溶液中某些镉(II)的混合配体配合物的稳定性研究: 关于混合配体配合物相对稳定性定量表征的讨论

本文用pH电位法研究了在70%(v/v)乙醇-水溶液中Cd(II)与维生素D3(VD3)和乙二胺(en)或2,2'-联吡啶(bipy)在37±0.1℃和离子强度为0.10(KNO3)条件下, 三元混配配合物的稳定性。结果表明, 上述混合配位体系均形成稳定的1:1:1型混配配合物, 且△logK值均为较大的正值(分别为+1.06和+1.54), 但相应的logX值却并不很大(分别为2.18和2.83)。从统计效应和配合物分子内的配体间疏水相互作用, 讨论了造成这种反应常结果的可能原因, 并针对如何判断三元混配配合物相对稳定性高低等问题提出了作者的见解。     

菲林B近红外分光光度法测定维生素C

在pH 3的三氯乙酸酸性介质中,菲林B可以定量地将还原型维生素C氧化成脱氢型维生素C,利用脱氢型维生素C在920 nm处有最大吸光度,测定其含量,建立了一种测定维生素C的新方法,并研究了影响反应的各种因素。该方法对维生素C的检出限为0.17 mg/L;线性范围为0.5~10 mg/L,对水果中维生素C含量测定的RSD<2.31%;回收率为99.7%~101.1%,比2,4-二硝基苯肼分光光度法测定结果的相对偏差<±1.6%。     

Ce3+对菠菜D1/D2/Cytb559复合物影响的光谱学研究

从Ce³⁺处理过的菠菜PSⅡ颗粒中纯化出了D1/D2/Cytb559复合物并研究了Ce³⁺对其光谱学性质的影响. 结果表明Ce³⁺处理过的菠菜生长发育改善, PSⅡ颗粒电子传递效率明显加快, D1/D2/Cytb559复合物UV-Vis 谱在Soret区和Q区分别蓝移3和2 nm; 荧光发射峰蓝移5 nm; EXAFS谱表明Ce³⁺已结合到D1/D2/Cytb559复合物上. 推测Ce³⁺已同时参与叶绿素卟啉环中N的配位和多肽氨基酸羧基氧的配位, Ce—N键长为0.253 nm, Ce—O键长为0.32 nm. CD谱表明Ce³⁺结合后其复合物二级结构未发生明显变化. 认为Ce³⁺加强了D1/D2/Cytb559复合物P680⁺原初电子供体的功能, 但对反应中心复合物的构象影响不大.     

(2S,3S,4R)-2-正戊基-3,4-二叠氮基四氢噻吩的合成

以（＋）－4，10－二氧杂三环[5.2.1.O^2,6]－癸－8－烯－3－醇为原料。经8步反应，对映选择性地合成出去氧维生素H的重要中间体：（2S，3S，4R）－2－正戊基－3，4－二叠氮基四氢噻吩。为对映选择性合成手性四氢噻吩类化合物提供了新的方法。     

D160大孔吸附树脂对染料木黄酮吸附性能的研究

研究了D160大孔吸附树脂对染料木黄酮的吸附性能.结果表明,在pH4.00时,该树脂对染料木黄酮有较好的吸附性能;静态饱和吸附容量为64.5mg/g树脂;用95%乙醇溶液作解吸剂,二次累计解吸率接近100%;表现速率常数k298=1.01×10-4s-1;测得吸附热力学参数分别为:△H=32.2kJ/mol,△S=119J/(mol·K),△G288=-2.03kJ/mol,△G298=-3.22kJ/mol,△G308=4.41kJ/mol.等温吸附服从Freundlich和Langmuir等温吸附规律;研究还表明,提高振荡频率对吸附有利.