气相色谱法分离和测定对甲硫基苯酚

采用气相色谱法分离和测定对甲硫苯酚。在Ф６ ×１ ．５ ×１ ５００ ｍ ｍ 玻璃柱内填充５ ％ Ｏ Ｖ１０１／ Ｃｈｒｏｍ ｏｓｏｒｂ Ｗ Ａ Ｗ Ｄ Ｍ Ｃ Ｓ 的色谱柱上,对甲硫基苯酚与内标物磷酸三丁酯及杂质之间具有较好的分离效果;而且以磷酸三丁酯为内标物时其重量校正因子相当稳定,即 ｆｗ ． Ａ ＝ ０ ．９４８ ±０ ．００５ ４（ｎ ＝ ９ ,α＝ ０ ．０５） 。该方法操作简便、快速、准确。对同一试样的８ 次平行独立测定其标准偏差为０ ．２５ ,变异系数为０ ．００７ ２ 。并且,该方法的３ 次加入法回收率达９８ ．１８ ％ ～９９ ．２２ ％ 。     

反相胶束增稳荧光法测定兔血浆中痕量盐酸小檗碱的研究

本文研究了气溶胶（ＡＯＴ）／环己烷／水反相胶束介质中中草药有效成分盐酸小檗碱的荧光性质,并将该法应用于兔血浆中痕量盐酸小檗碱的测定。该法的线性范围为１．０×１０－ ７～３×１０－ ５（ｇ／ｍ Ｌ）,检出限为８．３×１０－ ８（ｇ／ｍ Ｌ）,相对标准偏差为１．１％ 。     

分光光度法研究血清蛋白质与钍试剂Ⅰ的作用

钍试剂Ⅰ是测定无机离子的显色剂,在ｐＨ ３．８ 的Ｂｒｉｔｔｏｎ－Ｒｏｂｉｎｓｏｎ缓冲溶液中,该试剂能与血清蛋白质形成复合物,λｍ ａｘ为５３５ ｎｍ ,比试剂本身红移约５５ ｎｍ ,表观摩尔吸光系数为３．５６ ×１０５ Ｌ·ｍ ｏｌ－ １·ｃｍ － １（ＢＳＡ）,测定蛋白质的线性范围,为２０～１６０ ｍ ｇ／Ｌ。用于人血清样品总蛋白的测定,ＲＳＤ为１．０５ ％ （ｎ＝ ４）,回收率约为１００ ％ 。方法基本无干扰。     

铁,钴,镍的反相高效液相色谱分离和测定

１引言建立了用反相高效液相色谱同时测定铁、钴、镍的分析方法并对Ｍｅｎ＋－二硫腙（ＤＺ）体系的色谱行为进行了探索。较之萃取进样更快速、简便。测定条件为：Ｓｈｉｍ－ＰａｃｋＣＬＣ－ＯＤＳ（φ６×１５０ｍｍ，５μｍ）；流动相：甲醇：水：三氯甲烷（含１％三乙胺）（８０：１０：１０）；流速１ｍＬ／ｍｉｎ；柱温３５℃；检测波长２５４ｎ。线性范围０．０１－２．０ｍｇ／Ｌ；相关系数ｒ＝０．９９９ｌ～０．９９９８；检测限为０．００２３～０．００５０ｍｇ／Ｌ；相对标准偏差为１．８％－２．７％；回收率为９６％－１０４…     

薄层色谱法同时测定邻苯二酚、间苯二酚和对苯二酚异构体

研究了在自制硅胶薄板上邻苯二酚,间苯二酚异构体的薄层色谱特性。展开剂为本：乙醚：冰醋酸＝７：２：１（Ｖ／Ｖ／Ｖ）,Ｒｆ值分别为０．５９,０．５３,０．４８。检测限分别为１．０７×１０＾－４,１．６４×１０＾－４,１．９０×１０＾４ｍｏｌ／Ｌ。其他常见酚不干扰测定。可应用于实际样品的测定,回收率为９６％－１０４％。     

聚氯乙烯膜奎宁选择电极的研制与应用

本报道了一种以奎宁溴汞酸盐为电活性物的ＰＶＣ膜奎宁选择电极，其线性响应范围为１．０×１０＾－２－１．０×１０＾－６ｍｏｌ／Ｌ；级差５８±１ｍＶ；检测限为８．２×１０＾－７ｍｏｌ／Ｌ。以此电极测定奎宁的含量，方法简单、快速、结果与药典法相符。     

离子色谱法测定α—氧化铝中微量硫酸根的研究

本建立了用氢氧化钠溶样，离子色谱测定α－Ａｌ２Ｏ３中微量硫酸根的方法。在ＤｉｏｎｅｘＡＳ４Ａ分离柱上，用１．８×１０＾－＾３ｍｏｌ／ＬＡａ２ＣＯ３作流动相进行洗脱，电导检测器检测，分析方法简便，快速，硫酸根的检测限为１．０×１０＾－＾２μｇ／ｍｌ，相对标准偏差为２．６７％，回收率为９７．５％，扩展了离子色谱法测定实际样品的范围。     

鲁米诺-双氧水-铬(Ⅲ)化学发光体系测定化探样品中痕量砷

用鲁米诺－双氧水－铬（Ⅲ）化学发光体系结合巯基棉对Ａｓ（Ⅲ）的富集分离，建立了快速的测定化探样品中痕量砷的新方法，检测线性范围为１．０×１０－４～１．０×１０１ｍｇ／Ｌ，检出限为３．４×１０－５ｍｇ／Ｌ。用于实际化探样品测定，相对标准偏差为５．５％～９．０％。     

对甲苯磺酸正丁铵毛细管色谱柱的制备及性能考察

用动态涂敷法制备了对甲苯磺酸正丁铵玻璃毛细管柱柱１（固定液浓度为７．５％,柱尺寸为３５ｍ×０．３５ｍｍｉ．ｄ．）和柱２（固定液浓度为９．２％,柱尺寸为３５ｍ×０．３０ｍｍｉ．ｄ．）,所用溶剂是丙酮和甲醇（２：１Ｖ／Ｖ）的混合溶剂,并对柱性能进行了考察。结果表明,这种色谱固定相具有较强的极性并对饱和烃、芳香烃、饱和酸、芳香酸、极性异构体等具有良好的分离效果。     

HPLC法测定半纤维素水解液中糖的研究

研究了用ＨＰＬＣ分离测定毛竹水解液中的木糖、阿拉伯糖及葡萄糖等。探讨了试样的净化方法和分离条件，试样经活性炭和ＳｅｐＰａｋＧ８小柱净化，色谱柱为ＹＷＧ－ＮＨ２，１０μｍ，４．６×２５０，流动相为乙腈＋水＝８５＋１５，流量为０．８ｍＬ／ｍｉｎ，获最佳分离。木糖、阿拉伯糖、葡萄糖的平均回收率（％）分别为９９．１、１０１和９５．０，相对标准偏差为１．２５％、１．３９％和１．５３％。     

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.