从苦参中提取总生物碱的微型化学实验研究

采用常量法和微量法对苦参中的总生物碱进行提取,比较这2种方法在提取率、试剂用量和提取时间方面的不同。结果表明,微量法的提取效果略高于常量法,其提取率为0.565%;微量法的苦参用量是常量法的10%,所用试剂乙醇、氯仿、氨水只占常量法的30%左右;完成本次实验微量法共需要6.5 h,而常量法则需29 h。     

顺丁烯二酸酐的热失重动力学

顺丁烯二酸酐;等转化率法;主曲线法;热分析动力学     

HPLC与ELISA法测定牛奶中黄曲霉毒素M1的比较研究

对HPLC法和ELISA法检测牛奶样品中黄曲霉毒素M1(AFM1)残留量进行了比较,探讨了牛奶中黄曲霉毒素M1的最佳检测方法。结果显示,对于已知加标样品(阳性),HPLC法回收率为68%～85%;ELISA法回收率为97%～109%,HPLC法和ELISA法具有良好的相关性。ELISA法检验成本较低、检测迅速,但可能出现少量的假阳性和假阴性,故可用于待测样品的初筛;HPLC法检测结果准确,但检测费用较高,适用于黄曲霉毒素M1残留的确证。     

核磁共振法(NMR)和pH法研究Zn(Ⅱ)与HEDP(1-羟基乙叉-1,1-二膦酸)的配合物

本文用核磁共振法(NMR)和pH法对Zn(Ⅱ)与1-羟基乙叉-1,1-二膦酸(1-hydroxyethylidenel,1-diphosphonic acid,简称HEDP,以H₄L表示)的配合物进行了研究,由于pH<7时溶液中有沉淀生成,故NMR的研究是在溶液pH>7时进行.测定了溶液中不同Zn(Ⅱ)/HEDP摩尔比和pH值时³¹PNMR的化学位移。研究结果表明在pH7.5-11.0范围内生成Zn(Ⅱ)/HEDP=1(摩尔比)组成的配合物,在pH11.8-12.3范围内生成Zn(Ⅱ)/HEDP=2(摩尔比)组成的配合物,分别用pH法和NMR法测定了上述组成配合物的稳定常数.结果如下: logK_[zn(HL)^-] logK_[znL^2-] logK_[zn2L] pH法 4.69 7.51 11.63 NMR法——6.88-7.19 12.44.     

正常及肿瘤染色质的荧光寿命法、精确量热法和荧光能量转换

量热法;荧光寿命;正常及肿瘤染色质的荧光寿命法、精确量热法和荧光能量转换     

不同于教科书中的标准加入法——开放环境下授课的实例

为了加深学生对标准加入法（standard addition methods,SAM）的理解,将其列为“分析化学英文文献选读”选修课的一个专题,在学习资源开放、学习方式开放和学习结果开放的环境下,经过学习阶段、展示阶段和拓展阶段等密不可分的3阶段式问题导引下的主动学习和讨论,获得了有别于目前教科书内容的、鲜活的SAM内容：（1）由目前的2种类型拓展为9种类型的SAM;（2）由目前的外推法SAM拓展为内插法SAM;（3）由目前的容量法SAM拓展为重量法SAM;（4）新近出现的“稀释标准加入校准法”与这里讨论的SAM存在本质差别。在开放的环境下将传统的教学问题与新思路和新应用结合起来是一种行之有效的教学方法。它至少有以下3个优点：（1）以学生已有的知识为切入点,易于学生接受;（2）所选择的材料紧密跟踪分析化学的新进展,可以激发学生的兴趣;（3）课程以专题的形式展开,逻辑线索清晰。     

模板法室温合成CdS纳米棒

模板法室温合成CdS纳米棒;模板法;硫化镉;一维CdS纳米材料     

二季戊四醇的定量分析

采用两种不同的方法即重量法和杂质减除法对自行研制的二季戊四醇(简称二季或双季,DPE)进行了定值.重量法测得二季戊四醇的含量为98.97%,SD为0.078%;杂质减除法测得二季戊四醇的含量为98.79%,SD为0.092%;并进行了不等精度数据分析;结果表明这两种方法测得的结果是一致的.     

不同方法掺杂Au对纳米α-Fe2O3气敏性能的影响

分别采用共沉淀法、浸渍法、紫外辐照法制备了掺杂不同Au含量的α-Fe₂O₃纳米粉体, 并制作了旁热式厚膜型气敏元件. 用XRD、TG-DTA和TEM技术对纳米晶的晶型、晶粒大小及形貌进行了表征. 考察了掺杂方法、Au含量及焙烧温度对α-Fe₂O₃气敏性能的影响. 结果表明, 采用三种方法掺杂适量Au后, 都使α-Fe₂O₃的气敏性有了显著提高, 其中采用共沉淀法, 在400 ℃焙烧的Au质量分数为1.5％的α-Fe₂O₃的气敏性最佳.     

Cu(Ⅱ)-头孢曲松-赤藓红离子缔合物的UV-Vis、荧光和共振瑞利散射光谱分析及应用

头孢曲松钠;Cu(Ⅱ);赤藓红;共振瑞利散射法;分光光度法;荧光猝灭法     

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.