VPO催化剂的制备及其表征

采用ＢＥＴ、ＸＲＤ等测试手段,考察了由四种不同方法和条件下制备的ＶＰＯ催化剂的比表面积和晶体结构。实验结果表明：还原剂、溶剂、Ｐ／Ｖ、干燥条件及焙烧温度都对ＶＰＯ催化剂的物理性质有影响。水相法制备,获较复杂的晶相,且随着焙烧温度的提高样品的比表面积减小,晶相强度增加。有机相法制备,可获得较单一、活性好的晶相,且焙烧温度提高对样品的比表面积影响不大,但超临界条件下干燥,可使催化剂比表面积成倍地增大     

新显色剂对羧基苯基重氮氨基偶氮苯的合成及与镉显色反应的研究

本文报道了新色剂对羟基苯基重氮氨基偶氮苯的合成。     

Strategies for locating disulfide bonds in a monoclonal antibody via mass spectrometry

The location of the disulfide bonds in a recombinant monoclonal antibody was confirmed by matrix-assisted laser desorption/ionization-time-of-flight (MALDI-TOF) and electrospray ionization (ESI) mass spectrometry (MS). A non-reduced Endoproteinase Lys-C (Endo Lys-C) digest of the antibody was analyzed directly by MALDI-TOFMS. The sample was then reduced on-plate by depositing dithiothreitol (DTT) on the sample spot and re-analyzed by MALDI-TOFMS. The disulfide bonds were assigned based on the disappearance of certain mass ions in the non-reduced digest and the appearance of product ions in the reduced digest. A rapid LC/ESI-MS protocol was also developed to determine the location of the disulfide bonds. The peptides generated from the Endo Lys-C digest of the antibody were partially separated on a high performance liquid chromatography (HPLC) column by utilizing a steep gradient and analyzed by ESI-MS. The masses of the partially resolved peptides were determined by deconvoluting the mass spectra.     

ULTRASONICALLY DISPERSED POTASSIUM AS DEPROTONATING AND COUPLING AGENT──SYNTHESIS OF 1，6－DINITRILES IN SITU

ＵＬＴＲＡＳＯＮＩＣＡＬＬＹ　ＤＩＳＰＥＲＳＥＤ　ＰＯＴＡＳＳＩＵＭ　ＡＳ　ＤＥＰＲＯＴＯＮＡＴＩＮＧ　ＡＮＤ　ＣＯＵＰＬＩＮＧ　ＡＧＥＮＴ──ＳＹＮＴＨＥＳＩＳ　ＯＦ　１，６－ＤＩＮＩＴＲＩＬＥＳ　ＩＮ　ＳＩＴＵＵＬＴＲＡＳＯＮＩＣＡＬＬＹＤＩＳＰ...     

几种卟啉在化学还原沉积银膜上的表面增强拉曼光谱特征

应用 Ｊｏｂｉｎ－Ｙｖｏｎ Ｕ—１０００型拉曼光谱仪和ＬＡＢＲＡＭＩ型拉曼光谱系统研究了 ３种卟啉ＴＯＨＰＰ、ＴａｍＰＰ和ＴＳＰＰ在化学还原沉积法制备的银膜上的ＲＳ和ＳＥＲＳ光谱特征。结果表明：化学还原法制备的银膜可以作为这几种卟啉的拉曼增强活性载体。这３种卟啉在获谱的过程中都形成二聚态化合物和发生银离子搀和作用，较长的放置和测谱时间有利于银离子的搀和。     

Chiral Separation of Esmolol and Terazosin by Cyclodextrinmodified Capillary Zone Electrophoresis

IntroductionTheincreasingnecessity0fpharmacologicalresearchforchiraldrugshasrenderedchiralseparationanactiveareaincaPillaryelectroph0resis(CE)today.Variousmodes0fCE,includingcaPillaryzoneelectroph0resis(CZE),micellarelectrokineticchromatography(MEKC),caPillarygelelectrophoresis(CGE)andcapillaryisotachophoresis(CITP),havebeenappliedforthispurp0se',amongwhichCZEisthemostpopularoneforitshighefficiency,lowexpenseandeaseofoperation.Forsuccessfulchiralseparati0ninCZE,theselectortypeisofcr…     

ADSORPTION OF DYES ON ACTIVATED CARBON FIBERS

1.INTRODUCTIONDyewastewaterisakindofseriouspollutionsource.InthetraditionaltreatmentmethodsfordyewastewatergenerallytherearefourapproachesincludingelectricchargeneutraliZationofgelparticles,complexation(chelatation),redoxreaction,andbiochemicalcoagulationII~31.Recently,dyewastewaterhasbecomemoreconcentrated,moredifficulttodegradedbiochemically,andmorepoisonous,whichbringsaboutagreatchallengeforwatertreatment.AlthoughtheCOD(chemicaloxygendemand)mayfitthequalitystandardofwastewaterdischar…     

Photochemical naphthylation at(α-carbon atom of carbonyl and its equivalences

The photostimulated reaction of halonaphthalene with a series of carbanions derived from,propionic acid derivatives in liquid ammonia led to the naphthylation at a-carbon of the carbanions inan isolated yield ranging from 25％ to 86％.In all cases,the dehalonaphthalenes were found to,be by-products and the reaction was inhibited by p-dinitrobenzere.An electron transfer from thecarbanion to the halonaphthalene followed by ejection of halogen led to naphtbyl radical,as predictedby comparing the LUMOs of the carbanions and the halonaphthalenes,was involved in the process.Absence of the alkylnaphthalene and 1,2-dinaphthylalkane in the products indicates the smoothelectron transfer between(Naph-Nu)~+ and Naph-X.C-vs.O-naphthylation is fully addressed interms of MNDO calculations and acid-base principle.     

Stereoselectivity and nonmigratory insertion mechanism of dimethylacetylene dicarboxylate into metallocene-hydride of Cp2M(L)H [Cp = η5-C5H5; M = Nb,V; L = CO,P (OMe)3]: A DFT study

The insertion of an alkyne into transition metal–hydrogen bonds is a key elementary step in catalytic polymerization and hydrogenation processes. It was found that a (Z)- or (E)-type alkyenyl complex can be formed through trans/cis stereospecific processes. In this work, the reaction mechanism of Cp₂M(L)H [Cp = η⁵-C₅H₅; M = Nb, V; L = CO, P (OMe)₃] with dimethylacetylene dicarboxylate (DMAD), and the factors influencing the stereoselectivity have been investigated based on density functional theory calculations. The calculated results show that all of the reactions are exothermic. For L = CO, the Z-isomer product forms first even at low temperatures because of the low Gibbs free energy barrier (ΔG^#). Then the Z-pro converts to E-pro , while for L = P (OMe)₃, the exclusive product is the E-isomer. For different metal centers, the reaction mechanisms of the Cp₂M(CO)H + DMAD (M = Nb and V) reaction are similar, while their products are different at room temperature. For M = Nb, because the energy barrier of the isomerization from Z-pro to E-pro is low and the relative free energies of Z-pro and E-pro are almost equal, both Z-pro and E-pro can be obtained. While for the Cp₂V(CO)H + DMAD reaction, only the Z-pro can be obtained under mild conditions, E-pro can be obtained only at high temperatures. For the Cp₂M(CO)H+DMAD(M=V and Nb) reactions, the formation of E-isomer products proceeds via two five-membered ring transition states. The calculated results provide an reasonable explanation for the experimental results and predict a new insertion reaction.     

磁疗手术胆结石的红外光谱观测

本文报道用Nicolet 170 SXFT-IR红外光谱仪观测磁疗手术胆结石、磁疗破碎排出胆结石及服中草药破碎胆结石的红外光谱,分析并比较了它们的光谱特征。