全固态曲马多选择电极的研制与应用

报道了一种以曲马多碘化物与碘化铋的分子缔合物为电活性物的新型全固态选择电极,电极的能斯特响应范围为6.3×10~(-2)～3.2×10~(-5)mol·L~(-1),斜率为50mV/pC,检测限为0.6×10~(-5)mol·L~(-1)。此电极响应迅速,重现性好。用此电极以标准曲线法对注射液中的曲马多进行了测定,结果与紫外分光光度法相符。     

5—羟色胺敏感膜电极的研究 Ⅰ.离子缔合型5—羟色胺膜电极的研制

5-羟色胺(5-HT)与许多疾病的发生和发展有关。应用正交试验,研究了离子缔合型5-HT敏感膜电极的最优化膜组成。筛选了由3种定域体,7种增塑剂组成的213个配方,选定了以四苯硼-5-HT离子缔合物为活性物、磷酸三(2-乙基己基)酯为增塑剂的涂碳PVC膜电极。电极各项性能良好,其线性范围为1.00×10~(-2)～1.58×10~(-5)mol/L,检测下限为4.17×10~(-6)mol/L,斜率为59.7mV/p5-HT。电极寿命超过39天,用混合溶液法测定了体液中可能存在的17种物质的选择性系数。已用该电极测定了牛血小板中的5-HT。     

涂丝型PVC膜离子选择电极测定格列齐特缓释片

本文报道了以格列齐特碘化物与碘化铋形成的分子缔合物为电活性物的新型聚氯乙烯(PVC)膜格列齐特涂丝选择电极,电极的线性响应范围为2.1×10~(-6)~2.5×10~(-2)mol·L~(-1),级差电位为59m V/p C,检测限为1.6×10~(-7)mol·L~(-1)。该电极响应迅速,重现性好,用此电极测定了格列齐特缓释片的含量,方法简便,结果与药典法相符。     

涂丝型聚氯乙烯膜甲哌卡因选择电极的研制与应用

报导一种以甲哌卡因与碘分子缔合物为电活性物的新型全固态PVC膜甲哌卡因涂丝选择电极,电极的线性响应范围为1.0×10-1~8.1×10-5mol·L~(-1),级差为57m V/pC,检测限为4.32×10-5mol·L~(-1)。该电极响应迅速,重现性好,用此电极以标准曲线法对盐酸甲哌卡因注射液含量进行了测定,此法简便,结果与药典法相符。     

聚氯乙烯膜曲马多选择电极的研制与应用

报道一种以曲马多与四苯硼的缔合物为电活性物的新型PVC膜曲马多选择电极,电极的Nernst响应范围为1．0×10~(－2)~2．1×10~(－5)mol/L;斜率为57mV/pC;检测限为7．2×10~(-6)mol/L。此电极响应迅速,重视性好,用此电极以标准曲线法对药物中的曲马多进行了测定,此法简便,结果与紫外分光光度法相符。     

咖啡因离子选择性电极的研制及其用于测定可乐饮料中咖啡因

研制了以咖啡因-磷钼酸缔合物为电活性物质的离子选择性电极。试验表明:该离子选择性电极对咖啡因具有良好的选择性和电位响应特性。在pH 2.54磷酸盐缓冲溶液中,电极电位呈现能斯特响应,线性范围为5.0×10~(-6)～1.0×10~(-2)mol·L~(-1),斜率为51.4mV·pc~(-1)。将该电极用于测定可乐饮料中咖啡因的含量,测得方法的回收率在98.4%～102.4%之间。     

PVC膜黄连素离子选择电极的研制及应用

本文报道一种以黄连素溴汞酸盐为电活性物的涂碳型PVC膜黄连素离子选择电极,其线性响应范国为10~(-3)—5×10~(-7)mol/L,级差56mV(23℃),检测限为2.2×10~(-7)mol/L。应用此电极测定黄连素药片的含量,方法简单、快速,结果与药典法相符。     

功能高分子膜离子选择电极研究——Ⅲ.压片PVC膜氯离子选择电极的研制

用热压法制备了以功能高分子为活性物的PVC膜氯离子选择电极。合适的压膜温度为108—120℃,压力为50—130kg/cm~2。电极的线性范围1×10~(-1)～2×10~(-4)M,检测下限8×10~(-5)M,稳定性好,寿命长,适用pH范围宽,抗毒化能力强,响应快,内阻小。测定了电极内阻-活化时间曲线,认为活化过程同时是内阻降低至稳定的过程。     

聚氯乙烯膜盐酸地尔硫卓离子选择电极测定盐酸地尔硫卓

制备了一种以盐酸地尔硫卓与碘汞酸盐形成的缔合物为电活性物质的聚氯乙烯膜盐酸地尔硫卓选择电极,并对其性能做了测定,结果显示该电极对盐酸地尔硫卓有较好的能斯特响应。盐酸地尔硫卓的线性范围为4.5×10~(-2)～1.0×10~(-4)mol·L~(-1),检出限为3.55×10~(-5)mol·L~(-1)。该电极用于盐酸地尔硫卓片剂的分析,结果与药典法结果相符。     

基于三辛胺缔合作用的草酸及柠檬酸电极的制备

草酸、柠檬酸可分别与三辛胺(TOA)生成稳定的缔合物,化学分析和红外光谱表明缔合比为1∶1。以此缔合物为活性物质制作的PVC膜电极,测定溶液中的草酸盐、柠檬酸盐的线性范围分别为1.0×10-4~1.0×10-1mol.L-1和1.0×10-5~1.0×10-2mol.L-1。该电极用于简单模拟体系中草酸和柠檬酸浓度的测定,效果良好。     

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.     

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.     

Facile synthesis of bicyclic 1-arylpyrazol-5-ones

In this Letter, we described a facile method for constructing fused bicyclic 1-arylpyrazol-5-one ring system. We employed various methylene-containing carboxylic acids as the substrates and proved that the pyrazolone ring closure requires activated methylene group in intermediate II. Accordingly, a series of structurally diversified, fused bicyclic 1-arylpyrazol-5-ones was prepared in moderate to high yields using the requisite substrates.     

Synthesis of pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles by Curtius reaction in Morita-Baylis-Hillman derivatives

Synthesis of substituted pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles from the Morita-Baylis-Hillman derivatives of acrylates via saponification followed by Curtius reaction is described.     

正丁胺对激光染料荧光谱影响的研究

用正丁胺作为碳源,采用射频辉光放电制备碳膜,选用激光染料R6G和聚乙二醇混合液作为蒸气源,采用单源热蒸发,在蒸发室与染料同时沉积得到混合膜,用拉曼光谱和红外光谱分析了碳膜的结构和键合方式,分析表明:碳膜中存在胺基团和氢原子.混合膜的荧光谱测量结果表明,认为正丁胺对染料荧光谱的影响是因为胺基和氢原子的存在.     

Cu0-catalysed 1,3-dipolar cycloadditions of α-amino acid derived N,N-cyclic azomethine imines to ynones

A series of 20 CuAIAC reactions between eight 4-acylamino substituted pyrazolidine-3-one-1-azomethine imines and four terminal ynones were performed using Cu⁰ as catalyst. The corresponding fluorescent cycloadducts were obtained in very high yields upon simple workup. Thus, Cu-metal turned out to be a better catalyst than Cu^I in terms of yield and ease of isolation. Availability of azomethine imines, mild reaction conditions, and simple workup enable a “click” access to libraries of densely substituted 2,3-dihydro-1H,5H-pyrazolo[1,2-a]pyrazol-1-ones. Reactivity of differently substituted dipoles was evaluated experimentally and by quantum chemical methods (DFT).     

Synthesis and antioxidative/anti-inflammatory activity of novel fullerene–polyamine conjugates

(E)-4-(Fullerenopyrrolidin-1-yl)-3-methylbut-2-enoic acid and its corresponding succinimidyl ester, readily obtained through Prato-type modification of C₆₀, were used for the selective N-acylation of polyamines. The thus obtained conjugates were evaluated for their antioxidative and anti-inflammatory activity and their cytotoxicity was determined. Members of this family of compounds showed interesting anti-lipid peroxidation, anti-lipoxygenase and anti-inflammatory activity and comparable cytocompatibility to spermidine.