丙硫咪唑的离子／中性碎片复合物中间体质谱破裂

报道了丙硫咪唑（５－丙硫基－苯并咪唑－２氨基甲酸酯）的电子轰击质谱。利用串联质谱的低能碰撞诱导解离（ＣＩＤ）技术研究了此化合物的单分子解离，并提出了可能的离子／中性碎片复合筘间体碎裂机理，用来解释在质谱碎裂过程中出现的氢迁移（尤其是远距离的氢迁移）现象。     

丙硫咪唑的离子/中性碎片复合物中间体质谱碎裂

报道了丙硫咪唑（5-丙硫基-苯并咪唑-2-氨基甲酸甲酯）的电子轰击质谱。利用串联质谱的低能碰撞诱导解离（CID）技术研究了此化合物的单分子解离，并提出了可能的离子／中性碎片复合物中间体碎裂机理，用来解释在质谱碎裂过程中出现的氢迁移（尤其是远距离的氢迁移）现象。     

聚芳醚酮（砜）亚胺的裂解色谱质谱鉴定

本文通过对聚芳醚酮亚胺和聚芳醚砜亚胺两类聚合物的裂解色谱质谱的解析,归纳出适合于正确鉴定这两类新型聚合物的表征化合物。     

一些双电荷离子的气相碎裂反应

借助质量分析离子动能谱和串联质谱研究了由电子轰击产生的双电荷离子的单分子亚稳碎裂及碰撞诱导分解过程,讨论了两种实验方法导致的差别因素.此外,根据质量分析离子动能谱提供的双电荷离子电荷分离反应的动能释放值计算了两电荷中心间距的最小值,以判别按不同电荷分离方式碎裂的双电荷离子的过渡态结构.     

缩酚酸醚类化合物的电喷雾多级串联质谱研究

采用电喷雾多级质谱方法, 研究了三个从地衣中提取到的缩酚酸醚类化合物在电喷雾电离质谱中的裂解行为, 结果表明它们在电喷雾多级质谱中能得到较多碎片离子, 其裂解途径能体现它们的基本结构特征.     

系列新型咔哚聚芳醚砜结构的裂解色谱—质谱研究

利用裂解色谱－质谱对４个同一系列新型咔哚聚芳醚砜样品的裂解规律进行了研究，分别得到了各自链节的裂解特征碎片，证明了各聚合物确实发生了缩聚反应。     

苯乙酮碳苷化合物快原子轰击质谱的特征及碎裂机理的研究

采用正离子快原子轰击质谱(PFABMS)和联动扫描谱[1](B/E和B2/E)相结合,研究了六个苯乙酮-β-D-吡喃糖碳苷的裂解规律.不仅得到了各化合物的质子化分子离子峰[M+H+],而且通过联动扫描谱证实了此类化合物糖基序列特征离子的归宿,为研究此类碳苷化合物的结构提供了依据.     

含2—苯基—1,2,3—连三唑环的1,3,4—恶二唑衍生物的质谱研究

对两类非共轭的１，３，４－恶二唑衍生物Ⅰａ－３和Ⅱａ－ｅ的电子轰击质谱进行了研究，并通过Ｂ／Ｅ联动扫描对它们可能的裂解途径进行了探讨。     

2,5—双（4—羟基苯亚甲基）环戊酮中双电荷离子存在的串联质谱证据

应用串联质谱的碰撞诱导解离和联动扫描技术，研究了２，５－双（４－羟基苯亚甲基）环戊酮的质谱解离特征，提供了双电荷离子存在的实验证据。进一步对双电荷离子（ｍ／ｚ１４６）的碰撞诱导解离碎裂进行了讨论。     

低聚醚磺酸锂／梳形聚醚复合物的单离子导电性

低聚醚磺酸锂／梳形聚醚复合物的单离子导电性郑云贵，万国祥（中国科学院成都有机化学研究所成都６１００４１）关键词低聚醚磺酸锂，单离子导体，阳离子迁移数聚合物阳离子导体一般采用单体盐与能促进离子迁移的单体通过共聚或将其均聚物共混的方式制备’‘－‘’．由于...     

离子/中性复合物中间体研究进展

对离子/中性(碎片)复合物的形成、特征、反应、研究方法和近年来取得的重要成就及其应用进展进行了综述.简述了另一类特殊形式的离子/中性(碎片)复合物--质子键合复合物.     

LC/MSn法鉴定乙氧苯柳胺在家兔体内的主要代谢产物

报道了治疗痤疮新药乙氧苯柳胺［Ｎ－４－（乙氧苯基）－２－羟基苯甲酸胺］在家兔尿中的主要代谢产物．选择 ４只健康家兔,单剂量口服 ４００ ｍｇ乙氧苯柳胺,收集服药后 ０～１０ ｈ的尿样．将未经或经过β－Ｄ－葡萄糖苷酸酶／硫酸酯酶水解的尿样以固相萃取柱纯化后,采用 ＬＣ／ＭＳ~ｎ方法对尿中推测的代谢物和标准品分别进行选择离子监测（ＳＩＭ）和多级全扫描质谱（ＭＳ~ｎ）分析．结果在尿中发现了 ５个代谢物,分别为利胆酚［Ｎ－（对－羟基苯基）－水杨酰胺］以及利胆酚和乙氧苯柳胺与硫酸或葡糖醛酸的结合物．     

Synthesis,Characterization, Antimicrobial Activities,and Structural Studies of Lanthanide (III) Complexes with 1-(4-Chlorophenyl)-3-(4-fluoro/hydroxyphenyl)prop-2-en-1-thiosemicarbazone

Twelve coordinate lanthanide (III) complexes with the general composition [Ln L₃X_n(H₂O)_n] where Ln = Pr(III), Sm(III), Eu (III), Gd (III), Tb (III), Dy (III), X = Cl^?1, NO₃ ^?2, n = 2–7, and L is 1-(4-chlorophenyl)-3-(4-fluoro/hydroxyphenyl)prop-2-en-1- thiosemicarbazone have been prepared. The lanthanide complexes (5) were derived from the reaction between 1-(4-chlorophenyl)-3-(4-fluoro/hydroxyphenyl)prop-2-en-1-thiosemicarbazone (4) with an aqueous solution of lanthanide salt. Chalcone thiosemicarbazone ligand (4) was prepared by the reaction of [1-(4-chlorophenyl)-3-(4-fluoro/hydroxyphenyl)]prop-2-enone (chalcone) (3) with thiosemicarbazide in the presence of hot ethanol. All the lanthanide-ligand 1:3 complexes have been isolated in the solid state, are stable in air, and characterized on the basis of their elemental and spectral data.

Thiosemicarbazone ligands behave as bidentate ligands by coordinating through the sulfur of the isocyanide group and nitrogen of the cyanide residue. The probable structure for all the lanthanide complexes is also proposed. The chalcone thiosemicarbazone ligands and their lanthanide complexes have been screened for their antifungal and antibacterial studies. Some of the synthesized lanthanide complexes have shown enhanced activity compared with that of the free ligand.

Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements to view the free supplemental file.     

Potentiometric Studies of Some Bivalent Metal Ion Complexes of a New Ligand,o-(2-Thiazolylazo)-4-Ethylphenol

Abstract

The complexations of a new ligand, o-(2-thiazolylazo)-4-ethylphenol(TAEP) with Ca(II), Mn(II), Co(II), Ni(II), Cu(II), Zn(II), Cd(II), Hq(II) and Pb(II) have been studied by potentiometric titrations, at 25.0 ± 0.2°C and an ionic strength of 0.1 in 30% v/v dioxane-water mixture. The dissociation constant and spectral data of TAEP and formation constants of the complexes containing various molar ratios of metal ion to ligand, are reported. It is observed that Ca(II) forms only an ML complex in any molar ratios, whereas other metal ions react in two steps forming ML and ML₂ complexes in a 1:3 molar ratio. In the case of 1:1 and 1:2 molar ratios, Mn(II), Co(II), Cd(II) and Hg(II) seemed to form bi- or poly-nuclear complexes because of slightly different formation curves from those of 1:3 molar ratio. The sequence of the first successive formation constant is Cu > Hg > Ni > Pb > Co > Zn > Cd > Mn > Ca, showing Mellor-Maley's order. Further correlation is shown between the formation constants and the second ionization potentials of the metals.     

用离子抑制色谱法分析二(2,2,6,6-四甲基-4-哌啶基)马来酸酯合成反应液

建立了用离子抑制色谱法分析二（２,２,６,６－四甲基－４－哌啶基）马来酸酯合成反应液的方法。平均回收率为９８．８％,相对标准偏差为０．５６％,测量的平均相对偏差不大于５．０％。方法简单、快速,可用于工艺条件的选择和质量检测。     

Comparative Studies on Mass Spectrometric Fragmentation of Linear Chiral Secondary Alcohols （ R ） -1-（4-Alkylphenyl） and （ R ） -1- （ 4-Alkoxyphenyl/Alkylthiophenyl ） Alcohols

Introduction Chiralsecondaryalcoholsareveryimportantinter mediatesinorganicsynthesis.Theyaregenerallypre paredviachemicalorenzymaticresolutionofracemic secondaryalcohols[1—4],chemicalorenzymaticasym metricreductionofprochiralketones[5—7],andasym metrica…     

离子交换树脂相分光光度法测定铜

根据铜（Ⅱ）与１－（５－溴－２吡啶偶氮）－２蔡酚－６－磺酸（５－Ｂｒ－ＰＡＮ－Ｓ）形成稳定络合物这一性质,利用阴离子交换树脂为吸附载体,建立了离子交换树脂相分光光度法测定铜的新方法。以最大吸收波长５８４ｎｍ为测定波长,８００ｎｍ为参比波长,用双波长法进行测定,灵敏度高,选择性、重现性好。铜量在０￣１０μｇ范围内服从比尔定律,方法用于水样及人发中微量铜的测定,结果满意。     

Characterization of the Intermediate in and Identification of the Repair Mechanism of (6‐4) Photolesions by Photolyases

Quantum mechanics/molecular mechanics calculations are employed to assign previously recorded experimental spectroscopic signatures of the intermediates occurring during the photo‐induced repair of (6‐4) photolesions by photolyases to specific molecular structures. Based on this close comparison of experiment and theory it is demonstrated that the acting repair mechanism involves proton transfer from the protonated His365 to the N3′ nitrogen of the lesion, which proceeds simultaneously with intramolecular OH transfer along an oxetane‐like transition state.     

Structure elucidation of acetylation products of 2-acyl-1,3-indanediones by correlation of infrared spectral data

Summary 2-(1-Acetoxyalkylidene)- and 2-(1-acetoxybenzylidene)-1,3-indanediones (1a–1e) were proven to be the products of acetylation of 2-acyl-1,3-indanediones (2a–2e) by ketene using a detailed investigation and correlation analysis of infrared spectral data as well as¹H-NMR and¹³C-NMR spectra. Study by means of CNDO/2 and MMPI methods also demonstrates that the structure1 is more stable as the alternative one of 2-acyl-3-acetoxy-2-indene-1-ones (5). It was shown that the recently proposed general correlations v(C=O)_s vs. v(C=O)_as and v(C=O) vs. X⁺(R) as well as the mechanical anharmonicities of asymmetric C=O stretching vibration can be successfully used as a tool of structural diagnostics of cyclic 1,3-dicarbonyl compounds.

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Strukturaufklärung von Acetylierungsprodukten von 2-Acyl-1,3-indandionen mittels Korrelation von Infrarot-Daten

Zusammenfassung 2-(1-Acetoxyalkyliden)- und 2-(1-Acetoxybenzyliden)-1,3-indandione (1a–1e) wurden mittels einer detaillierten infrarot-spektroskopischen Untersuchung (IR-Korrelation) und¹H-NMR und¹³C-NMR Spektroskopie als Acetylierungsprodukte von 2-Acyl-1,3-indandionen (2a–2e) mit Keten nachgewiesen. CNDO/2- und MMPI-Rechnungen zeigten auch, daß Struktur1 stabiler ist, als die der alternativen 2-Acyl-3-acetoxy-2-inden-1-one5. Es wird gezeigt, daß die kürzlich vorgeschlagenen allgemeinen Korrelationen v(C=O)_s gengen v(C=O)_as und v(C=O) gegen X ⁺(R) und auch die mechanischen Anharmonizitäten der asymmetrischen C=O Streckschwingung erfolgreich als Werkzeug zur Strukturaufklärung cyclischer 1,3-Dicarbonyl-Verbindungen eingesetzt werden können.