流动注射化学发光法测定盐酸异丙嗪

在酸性溶液中，高锰酸钾能氧化盐酸异丙嗪产生化学发光反应，乙二醛的存在可使发光强度增强。据此，采用流动注射技术，建立了一种测定盐酸异丙嗪的化学发光分析分析。方法的检出限为３．５×１０＾－８ｇ／ｍＬ，相对标准偏差为２．８％（１．０×１０＾－６ｇ／ｍＬ盐酸异丙嗪，ｎ＝１１），线性范围为１．０×１０＾－７￣６．０×１０＾－５ｇ／ｍＬ。该法已用于盐酸异丙嗪针剂和片剂中盐酸异丙嗪含量的测定，并与药典标准方法进     

高效液相色谱法测定盐酸芬氟拉明及其在片剂中含量

应用高效液相色谱法测定了盐酸芬氟拉明及其片剂的含量,使用２５ｃｍ×０．４６ｃｍｉ．ｄ．分析柱,填充ＨｙｐｅｒｓｉｌＢＤＳＣ１８（５μｍ）,检测波长２６４ｎｍ,流动相为Ｖ（乙腈）∶Ｖ（０．４ｍｏｌ／Ｌ乙酸铵）∶Ｖ（三乙胺）＝３０∶７０∶２。选用咖啡因作内标物,用内标法进行定量测定,在０．１～０．５ｇ／Ｌ范围内呈良好的线性关系,相关系数为０．９９９９。片剂的平均回收率为９９．９８％。方法简单、快速、灵敏度高、重现性好。     

高效液相色谱法检测人血浆中安定及其代谢产物的浓度

建立一种快速测定人血浆中安定与去甲安定的反相液相色谱方法,采用ＳｐｈｅｒｉｓｏｒｂＯＤＳ２柱及甲醇：水（１００：６５）作流动相,ＵＶ检测波长２２９ｎｍ,流速１．２ｍＬ／ｍｉｎ,卡马西平作内标。线性范围０．００５～１００ｍｇ／Ｌ,相对回收率为（９９．１±５．６）％（安定）及（９９．０±６．８）％（去甲安定）,检测极限２μｇ／Ｌ。日内和日间变异系数分别为４．１％（安定）、５．４％（去甲安定）和５．１％（安定）、５．８％（去甲安定）。     

荧光光度法直接测定环境水中的苯酚和苯胺

了用荧光分光光度法通过控制酸度直接测定环境水中苯酚和苯胺两种水中污染物的新方法。在ｐＨ＝１时，直接测定苯酚的含量，波长为λｅｘ／λｅｍ＝２７０／２９７ｎｍ，检出限为４．０ｎｇ／ｍＬ，线性范围为０～３．２μｇ／ｍＬ。在ｐＨ＝１２时，直接测定苯胺的含量，波长为λｅｘ／λｅｍ＝２８０／３４０ｎｍ检出限为４．３ｎｇ／ｍＬ，线性范围为０～２．０ｕｇ／ｍＬ，回收率达９９～１０１％。     

流动注射光化学荧光法测定药物制剂中的盐酸氯丙嗪

氯丙嗪的流动注射光化学反应在一编结反应器中进行，该反应器盘绕在一荧光灯上并接受由该灯发生出的最大幅波长为３６５ｎｍ的紫外线照射。用２５３．０ｎｍ的激发波长和３７４．５ｎｍ的荧光波长在线测定光化学反应产物的荧光强度。在最佳条件下，检测限为５．４μｇ／Ｌ，采样速度为９０次／ｈ，１ｍｇ／Ｌ的分析物１１次测定的相对标准偏差为０．５％，动态线性范围为０．０１－６．００ｍｇ／Ｌ。所建立的方法已成功地地用于片剂     

荧光光度法快速测定片剂中氨酰心安的含量

研究了氨酰心安的荧光光度法，其最大激发波长和荧光波长分别为２２２．３ｎｍ和２９７．４ｎｍ。该法灵敏度高，操作简便，氨酰心安浓度在０～３．００μｇ／ｍＬ范围内与相对荧光强度呈线性关系，相关系数为０．９９９７，检测限为０．０１６９μｇ／ｍＬ。该法用于测定片剂中氨酰心安含量，结果满意。     

阿斯美胶囊中四种组分的高效液相色谱分析

建立了反相高效液相色谱法测定阿斯美胶囊中氨茶碱、盐酸甲氧非那明、马来酸氯苯那敏及那可汀四种组分的含量。色谱柱为ＳｐｈｅｒｉｓｏｒｂＣ８，５μｍ，２００ｃｍ×４０ｍｍＩＤ，流动相为体积分数０５％的三乙胺溶液（磷酸调节ｐＨ５５）＋乙腈＋甲醇（５５０＋３６８＋８２），检测波长为２６４ｎｍ，线性范围分别为：氨茶碱３１２５～２５０ｍｇ／Ｌ，γ＝０９９９６，盐酸甲氧非那明１５６２５～１２５０ｍｇ／Ｌ，γ＝１００００，马来酸氯苯那敏２５～２００ｍｇ／Ｌ，γ＝０９９９９，那可汀８７５～７００ｍｇ／Ｌ，γ＝０９９９９；回收率（ｎ＝３）分别为１０１２％，１００８％，９９９％，９９５％；精密度：日内平均ＲＳＤ（ｎ＝６）分别为０７％，０４％，０４％，０６％；日间平均ＲＳＤ（ｎ＝３）分别为１０％，１０％，１１％，１２％。     

反相离子对色谱法测定制剂中的舒必利

建立了反相离子对色谱用于测定制剂中舒必利的含量。采用Ｃ８柱，流动相为３５％甲醇－６５％的０．１ｍｏｌ／Ｌ甲酸铵缓冲液（含已烷磺酸钠，ｐＨ＝３．５），检测器ＵＶ２９０ｎｍ，片剂中舒必利平均回收率为９８．８８％￣１００．９２％，样品测试日内及日间ＲＳＤ分别为１．０４％￣２．２９％及１．８５％￣３．０２％。     

双波长吸光度比值K系数法同时测定三组分体系的研究与应用

本文用双波长吸光度比值Ｋ系数法同时测定撒痛风注射液中水杨酸钠，咖啡因和安替比林三组分的含量，其平均回收率及变异系数分别为１０１．５％，０．４０％；９９．９９％，０．３７％；１００．０％，０．３０％。既改善了选择性，又提高了灵敏度，弥补了常规Ｋ系数法的不足。     

高锰酸钾氧化—荧光分光光度法测定片剂中叶酸含量

以ＫＭｎＯ４为氧化剂,在ＰＨ４．２,８０℃水浴条件下,以２８９ｎｍ为激发波长,在４４０ｎｍ处测定叶酸氧化产物喋呤－６－羧酸的荧光强度,从而间接测定叶酸的含量,叶酸的检测限为０．７４μｇ／Ｌ,较直接荧光法测定叶酸的灵敏度提高了１２．５ｗｕｋ。利用本法测定叶酸片剂的含量,回收率为１０３．３％－１１４．０％之间,相对标准偏差小于１．８％。     

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.