3种分光光度法对天然抗氧化物质抗自由基性能的分析检测

用1,1 二苯基 2 苦基肼(DPPH)自由基捕获、亚硝基R盐 Co3 褪色、连苯三酚红等3种分光光度法对3种野生植物抗氧化剂的对自由基的作用进行了分析检测及方法比较研究。3种分光光度法对自由基的分析检测及抗氧化剂的抗自由基性能检测方法,对于普通实验室检测自由基或相关的研究工作具有很好的实用性。没食子酸丙酯及葡萄籽提取物的抗氧化性要优于灯盏花素提取物。对自由基的清除率可以达到40%～80%,具有很好的抗氧化能力及氧自由基清除作用。     

抗氧化剂的毛细管电泳-间接化学发光联用在线评价方法研究

根据碱性条件下羟自由基与luminol反应会产生化学发光而抗氧化剂能够清除羟自由基从而抑制发光的原理, 结合毛细管电泳技术, 建立了一种针对多组分共存体系中抗氧化组分的在线评价的新方法. 对这种毛细管电泳-间接化学发光检测技术, 优化化学发光的各种条件, 考察了抗氧化剂硫脲和麻黄碱的抗氧化活性, 采用曲线拟合求出它们对羟自由基的半数清除浓度(IC₅₀), 得出抗氧化活性大小为麻黄碱＞硫脲, 这与荧光分光光度法的结果一致. 该方法初步应用于评价中药槐米提取物化学组分的抗氧化活性.     

罗丹明B-Mn2+-H2O2体系同步荧光分光光度法测定中药的抗氧化活性

罗丹明B能产生特征荧光,其激发波长和发射波长分别为554 nm和575 nm。弱碱性介质中Mn2 -H2O2体系产生的羟自由基可迅速氧化罗丹明B使荧光猝灭,而中药水提取物可部分清除溶液中羟自由基,从而使其荧光猝灭程度减弱。用Δλ=21 nm的同步荧光分光光度法建立了测定中药抗氧化活性的方法。测试了11种中药的抗氧化活性,以五倍子的抗氧化活性最强。     

鸡足山耳蕨总黄酮的提取及抗氧化性研究

研究鸡足山耳蕨中总黄酮的提取及其抗氧化性.采用70％乙醇提取鸡足山耳蕨中总黄酮,用NaNO2Al(NO3)3-NaOH分光光度法测定黄酮含量,将提取液采用Fenton体系、普鲁士蓝法进行体外抗氧化活性研究,用硫代巴比妥酸(TBA)分光光度法研究其对羟自由基·OH引发DNA氧化损伤的抑制作用.结果表明样品中总黄酮含量为4.98％,回收率99.78％( RSD=1.06％,n=5).总黄酮浓度为90μg/mL时,对·OH的清除率可达36.2％;浓度为87.5μg/mL时,对羟自由基引发DNA损伤的抑制率可达93.0％.说明鸡足山蕨中总黄酮对羟自由基有较好的清除能力,对DNA氧化损伤有显著抑制作用.     

黄酮的研究现状

黄酮是存在于自然界中的一大类物质。黄酮的提取方法主要有微波、超声波、酶解、浸提和超临界萃取等。一般采用硅胶过柱分离、颜色法进行定性检测,HPLC和紫外分光光度法进行定量检测。黄酮活性的测定主要是测其抗氧化性能。     

基于手机光线传感器为检测器的简易光度计的自组装设计

利用手机光线传感器作为检测器搭建了一套可用于定量分析实验的简易光度计,将其用于邻二氮菲分光光度法测定铁的实验,进行了5次平行实验,每次实验拟合直线的R²值在0.999左右,待测样品中铁含量的RSD值为2.81%。将简易光度计用于邻二氮菲分光光度法测定铁的实验并与分光光度法进行对比,待测物铁含量分别为5.11和4.94μg·mL^-1。利用手机光线传感器作为检测器的自组装光度计实验,简单、方便、准确、易于实现,可替代传统的分光光度计;通过搭建简易光度计并进行测定实验,有利于增强学生对分光光度计的结构和原理的理解,激发学生的学习兴趣,提高实验教学的质量。     

水中六价铬分析方法研究进展

对近年来水中六价铬的检测方法进行了综述,包括分光光度法、原子吸收分光光度法、离子色谱及其联用法、液相色谱及其联用法。对几种检测方法进行分析,展望了六价铬测定方法的发展方向。     

环境样品检测中总氮值低于氨氮值的探讨

正总氮和氨氮是反映水体富营养化程度的重要指标,也是地表水、生活污水和工业废水监测中的常规分析项目。目前,在我国环境监测领域中,水质总氮的测定多采用碱性过硫酸钾消解紫外分光光度法[1],水质氨氮的测定多采用纳氏试剂分光光度法[2]。理论上,同一样品的总氮测定值应大于氨氮测定值,然而在实际的监测工作中发现:氨氮、硝酸盐氮和亚硝酸盐氮的测定总和大于总氮,甚至氨氮的测定值高于总氮测定值。采用不同检测方法进行对     

近红外光谱结合化学计量学快速测定羊栖菜抗氧化活性

基于近红外光谱技术建立了快速、高效的羊栖菜抗氧化活性评价方法。采用紫外-可见分光光度法测定了6批共150个羊栖菜样本的抗氧化活性,包括1,1-二苯基-2-三硝基苯肼（DPPH）自由基清除能力、2,2’-联氮-双-3-乙基苯并噻唑啉-6-磺酸（ABTS）自由基清除能力和铁离子还原能力（FRAP法）。采用NIRS和偏最小二乘法（PLS）建立了3个抗氧化活性指标的定量校正模型,并采用不同光谱预处理方法和竞争性自适应重加权采样（CARS）方法优化模型性能。将校正集相关系数（RC）、预测集相关系数（RP）、校正集均方根误差（RMSEC）和预测集均方根误差（RMSEP）作为校正模型的评价指标。结果表明,3个定量校正模型的预测精度均较理想,RP和RMSEP分别为0.968和2.42%、0.967和0.73%、0.979和3.60μmol/L。基于NIRS和CARSPLS所构建的方法可以成功用于羊栖菜的抗氧化活性测定,具备分析快速、操作简便、经济环保的优点,对保障羊栖菜品质、提升羊栖菜品质控制水平有一定的指导意义。     

用电化学方法研究红景天和丹参清除超氧阴离子自由基和羟基自由基的作用

利用单扫示波极谱法研究了红景天和丹参对活性氧自由基(O_2~-,OH)的清除作用.超氧阴离子自由基(O_2~-)通过邻苯三酚自氧化体系产生.羟基自由基由Fenton反应生成,用自旋捕集剂苯基叔丁基氮酮(PBN)捕捉生成的OH,以单扫示波极谱法检测自旋加合物.红景天和丹参样品对O_2~-和OH均有一定的清除作用,丹参对活性氧自由基的清除作用强于红景天.对O_2~-的清除能力为:红景天甙>吉林长白山红景天>西藏红景天;丹参对照品>安国丹参(Ⅰ)>安国丹参(Ⅱ).对OH的清除能力为:红景天甙>吉林长白山红景天>西藏红景天;安国丹参(Ⅱ)>安国丹参(Ⅰ)>丹参对照品.分别计算了各样品对自由基清除作用的IC_(50)值.     

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.     

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.     

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.     

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.     

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.     

Sulfur-directed metal-free and regiospecific methyl C(sp3)–H imidation of thioanisoles

Regiospecific and direct imidation of the methyl C(sp³)–H bond of thioanisoles is realized under mild and metal-free conditions with N-fluorobis(benzenesulfonyl)imide as an oxidant and nitrogen source. Proposed mechanism suggests that thionium ion intermediates and a Pummerer-type reaction are involved. The imidation has advantages such as high step-economy, excellent functionality tolerance, and regiospecificity, giving structurally diverse imidation products.     

Selective syntheses of 2H-1,3-oxazines and 1H-pyrrol-3(2H)-ones via temperature-dependent Rh(II)-carbenoid-mediated 2H-azirine-ring expansion

The Rh(II)-catalyzed reaction of 2-carbonyl-substituted 2H-azirines with ethyl 2-cyano-2-diazoacetate or 2-diazo-3,3,3-trifluoropropionate provides an easy access to 2H-1,3-oxazines and 1H-pyrrol-3(2H)-ones. These compounds can be selectively prepared from the same starting material using temperature as the only varied parameter. The 2-azabuta-1,3-diene intermediate, a common precursor for both heterocyclic products, isomerizes into 2H-1,3-oxazine under kinetic control, while 1H-pyrrol-3(2H)-one is the sole product of the reaction at elevated temperatures. According to DFT-calculations a one-atom oxazine ring contraction involving ring-opening to a 2-azabuta-1,3-diene intermediate, followed by a 1,5- and 1,2-prototropic shift leads to the consecutive formation of imidoylketene and azomethine ylide, which then further undergo cyclization to the pyrrole derivative.     

Synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives

Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields.