活血化瘀中药中无机元素含量测定

采用原子吸收分光光度法测定了丹参、红花草、益母草等活血化瘀中草药中多种无机元素的含量。结果表明,这些中草药中含有多种直接参与组织代谢的微量元素。     

饲料中含硒量的差异对动物体内硒含量的影响

用原子吸收分光光度法测定了普通饲料、低 硒饲料之间的硒含量的差别以及在这两种条件饲养下长大的大鼠血硒含量。结果表明,饲料中硒含量的差异对动物体内硒含量具有较大影响。     

富硒金针菇子实体中硒多糖的分离纯化技术及红外光谱研究

对富硒金针菇子实体中硒多糖(Se-containing polysaccharide,Se-P)的分离、纯化进行了优化研究,并采用苯酚-硫酸法、ICP-MS法对硒多糖中多糖及硒含量进行了测定.确定硒多糖的最佳提取条件为:浸提温度80℃、浸提时间3 h、料液比1:50、提取3次合并滤液;其中多糖含量为12.48%,硒含量为7.97μg/g.将粗多糖经Sephadex G-100柱层析系统分离纯化,所得精硒多糖进行红外光谱分析表明:可溶性硒多糖均为糖苷键连接的吡喃多糖,其中水溶性硒多糖与普通多糖结构相似,而碱溶性硒多糖中由于硒酸酯的形成改变了原有多糖的吡喃环糖苷键的构型,进一步证明在金针菇的富硒培养过程中,硒参与了硒多糖的合成.     

催化动力学光度法测定抗癌中草药中痕量硒

研究了硒催化溴酸钾氧化甲基橙反应体系测定痕量硒的方法,并探索了该反应的动力学条件。硒浓度在0.8-8.4μg·L-1范围内与Ig(A。／A)呈线性关系,方法灵敏度为0.687μg·L-1。用于抗癌中草药中硒的测定,结果满意。     

外源性加硒法增加枣中硒含量的研究

以不同深度硒溶液对枣树进行不同次数的叶面喷施,得到了不同硒含量的枣样品,用荧光光度法测定了样品中硒的含量。结果表明,与对照组相比,用外源性加硒法可明显提高枣中硒的含量;并且可通过调节喷施液浓度和喷施次数,得到硒含量适宜的成熟小枣。     

微量元素硒的检测方法进展

介绍了硒的各种检测方法，报道了它们在中草药、食品、环境和生物样品中的应用和检测结果．     

克山病病区硒水平监测的10年总结

对陕西省黄陵县克山病病工欠群内外环境硒水平进行了１０年动态监测。结果表明：①当地产小麦、大米、玉米和黄豆硒含量监测是无明显变化,均仍低于非病区同种粮食硒水平,病区居民所食外地麦面硒含量明显高于当地产小麦硒含量;②病区儿童发硒含量明显上升并已达到非病区水平;③病区人群内环境硒水平提高。可能与食用外地表现和硒磺盐有关。     

豆腐生产过程中微量元素硒分布特性研究

为确定以不同硒含量的大豆为原料生产豆腐过程中硒分布特性,用石墨炉原子吸收分光光度法对该过程中各种产物的硒含量进行了分析研究。结果表明,以硒含量分别为0.692、2.561、2.801 mg/kg的大豆为原料生产得到的豆腐、黄浆水、豆渣的硒含量分别为:0.089、0.250、0.138 mg/kg,0.462、0.760、0.507 mg/kg和0.532、0.764、0.524 mg/kg。豆腐生产过程中,以低硒大豆为原料生产豆腐,硒总回收率为75.59%;采用富硒大豆为原料生产,硒的回收率分别达到87.37%、87.20%;生产过程中豆腐、黄浆水和豆渣中硒含量占总回收硒的比率分别为39.01%～49.97%、23.92%～29.89%、26.11%～30.92%。     

硒酵母中有机硒及硒代氨基酸含量的测定方法

报道了人工培养硒酵母中有机硒及硒代胱氨酸（ＳｅＣｙｓ）和硒代蛋氨酸（ＳｅＭｅｔ）含量的测定方法。采用透析处理法使硒酵母中的无机硒和有机硒得以分离,并采用催化分光光度法测定了硒酵母中有机硒的含量;采用氨基酸自动分析仪测定了硒酵母中ＳｅＣｙｓ和ＳｅＭｅｔ的含量。     

隆回富硒区山银花不同花期硒分布规律研究

通过分析山银花不同花期硒含量,探讨了山银花中硒的积蓄规律与土壤硒之间的关系。选择湖南省隆回县小沙江地区加油站北和岩背村两处土壤硒含量分别为0.968 mg/kg和0.837mg/kg的山地,种植灰毡毛忍冬的两个不同品种:白云一号和金蕾一号,在花期内连续采收绿蕾期、白蕾期、白花期和金花期样本,脱水后,用电化学法测定硒含量。结果表明,白云一号和金蕾一号的绿蕾期、白蕾期、白花期和金花期硒平均含量分别为0.111、0.191、0.191、0.295 mg/kg和0.146、0.260、0.272、0.363 mg/kg,金蕾一号的硒积蓄能力优于白云一号。结论是富硒区山银花中硒的积蓄量与品种、花期密切相关,但与土壤中硒含量无明显相关性。     

二氧化碳和丙烯直接合成甲基丙烯酸的NiPMo/TiO2催化剂的研究

用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%.     

Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction

In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments.     

α-Amino acid derived enaminones and their application in the synthesis of N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates and other heterocycles

A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives.     

Specific intramolecular aromatic CH insertion of diazosulfonamides

The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp³)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp²)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp²)?H and aliphatic 1,5- and 1,6-C(sp³)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp³)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp²)?H insertion.     

CoFe2O4自形成磁性液体场致结构化对磁化的影响

The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula.     

KMnO4-mediated oxidative CN bond cleavage of tertiary amines: Synthesis of amides and sulfonamides

KMnO₄-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields.     

Highly regioselective Buchwald–Hartwig amination at C-2 of 2,4-dichloropyridine enabling a novel approach to 2,4-bisanilinopyridine (BAPyd) libraries

The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines.     

Chemistry of heterocyclic compounds at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences, over 50 years (Review)

The review contains a concise historical account and information on the most significant researches undertaken by the staff at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry of Heterocyclic Compounds. Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008.     

N-Heterocyclic carbene-palladacyclic complexes: synthesis,characterization and their applications in the C-N coupling and α-arylation of ketones using aryl chlorides

N-Heterocyclic carbene-palladacyclic complexes 3 were successfully achieved in a one-pot procedure under mild conditions. The structure of 3a was unambiguously confirmed by X-ray single crystal diffraction and it was an active catalyst in the Buchwald-Hartwig amination and α-arylation of ketones even at very low catalyst loadings (0.01?mol%).     

Iodine-mediated oxidative Pictet-Spengler reaction using terminal alkyne as the 2-oxoaldehyde surrogate for the synthesis of 1-aroyl-β-carbolines and fused-nitrogen heterocycles

An efficient iodine-mediated oxidative Pictet-Spengler reaction in dimethyl sulphoxide (DMSO) using terminal alkynes as the 2-oxoaldehyde surrogate for the synthesis of aryl (9H-pyrido[3,4-b]indol-1-yl)methanones is described. The scope of the protocol includes the total synthesis of Fascaplysin, Eudistomins Y₁ and Y₂. The methodology is extended for preparing pyrrolo[1,2-a]-quinoxaline and indolo[1,5-a]quinoxaline derivatives. The utility of 1-aroyl-β-carbolines was demonstrated by performing palladium-catalyzed β-carboline directed ortho-C(sp2)-H functionalization of the phenyl ring with thiomethyl (SMe) group using DMSO as source and for accessing 4-aryl-canthin-6-ones.