槟榔中槟榔碱和槟榔次碱的毛细管电泳分析

建立了槟榔中槟榔碱和槟榔次碱的毛细管电泳分析方法。考察了电解质溶液ｐＨ值变化对分离的影响,在选定实验条件下,槟榔碱和槟榔次碱得到了很好的分离,整个分析过程在１０ｍｉｎ内完成,其中槟榔碱和槟榔次碱的迁移时间相对标准偏差在０．４％￣０．７％之间,峰面积的相对标准偏差在３．４％￣３．８％之间。用于实际样品测定,结果满意。     

液相色谱法测定槟榔饮片中槟榔碱含量的不确定度评定

根据《测量不确定度评定与表示》对液相色谱法测定槟榔饮片中槟榔碱含量的不确定度进行评定。通过分析得出,体积类不确定度是主要影响因素。分析结果表明,当槟榔饮片中槟榔碱含量为0．58％时,其扩展不确定度为0．02％（k=2）     

植物生物分子的电分析化学研究X槟榔碱电化学行为及测定

槟榔碱主要存在于棕榈科植物槟榔的种子内。槟榔是我国目前亟待开发的天然植物资源,广泛分布于海南、广西、云南、福建及台湾等地。槟榔碱味辛、温,具有杀虫、破积、下气、行水的功能。由于槟榔碱对M—胆碱受体的作用,平时嚼食槟榔,可促使唾液分泌增加、增进     

海南产槟榔、沉香及槟榔-沉香药对中锰的测定与生物利用性

为测定海南产槟榔、沉香及槟榔-沉香(质量比为1∶1)药对中锰的含量与生物利用性,并了解锰的健康效应,采用火焰原子吸收光谱法(FAAS)测定了槟榔、沉香原药及其水煎液中锰的含量,并用体外消化-透析法模拟人体胃肠道消化,研究了锰的生物利用性.结果表明,该法回收率为98.32%～102.40%,RSD为1.24%～1.76%...     

槟榔提取物中多酚含量的测定

考察了福林酚试液用量、Na_2CO_3溶液用量、反应时间等因素对槟榔提取物中多酚测定的影响,确定了多酚测定条件,建立了测定槟榔提取物中多酚的方法.结果表明,在选定的测定条件下,没食子酸浓度在2.0～10.0 mg/L之间与吸光度成良好线性关系.线性方程为:y=0.103 8x-0.067 6;相关系数r=0.999 5;检测限为0.026 mg/L.该方法具有仪器简单、操作简便,准确度高等特点,用于槟榔提取物中多酚的测定,结果满意.     

薄层色谱法检测槟榔中糖精含量

在湖南长沙、湘潭等地素有嚼食槟榔的传统习惯,每年要消耗槟榔干果数10t.槟榔在精制过程中,常加入糖精以增加甜度.作为化工产品的糖精,毫无营养价值,对人的致癌性目前尚有争论.我国食品中糖精限量一般为不超过0.159·kg~(-1),故检测槟榔中糖精含量有卫生学意义.糖精的测定方法目前有薄层色谱法、电极法、比色法、紫外光谱法、高压液相色谱法等.但是较简便的方法还是首推薄层色谱法,该法是测定食品中糖精的国标法.我们在已有工作的基础上,参照国标法,选用硅胶GF_(254)作吸附剂,测定了210件槟榔样品中糖精含量,结果满意.     

高效液相色谱-串联质谱法测定食用槟榔中4种黄曲霉毒素的含量北大核心CSCD

将粉碎后的槟榔样品2.00g用20mL乙腈提取,以100mg N-丙基乙二胺为净化剂分散固相萃取净化萃取液。取上清液以Thermo Accucore aQ C18色谱柱为固定相,以0.005mol·L-1乙酸铵溶液-乙腈混合液为流动相进行梯度洗脱,采用高效液相色谱-串联质谱法测定其中4种黄曲霉毒素的含量。质谱分析中采用电喷雾离子源和多反应监测模式。结果表明:4种黄曲霉毒素的质量浓度均在0.1～10.0μg·L-1内与其峰面积呈线性关系,测定下限(10S/N)为1μg·kg-1。以食用槟榔样品为基质,按标准加入法进行回收试验,回收率为80.0%～99.2%,测定值的相对标准偏差(n=6)为1.5%～9.3%。     

含噻二唑硫醚的槟榔碱新衍生物的合成及舒张血管活性

槟榔碱衍生物;四氢吡啶;噻二唑;合成;舒张血管活性     

引种地、采收期及药用部位对槟榔微量元素含量的影响

以等离子体发射光谱法测定了槟榔中２０种微量元素含量．结果表明，广州产槟榔所含１１种人体必需微量元素含量与进口摈榔接近，Ｐｂ、Ｃｄ、Ａｓ含量较低．槟榔不同部位微量元素含量均有显著差异。未成熟的槟榔种子微量元素含量与成熟种子有显著差异，其Ｐｈ含量达２．２１×１０－６，为成熟种子Ｐｂ含量的２０倍。     

丁二酮肟分光光度法测定大气颗粒物中的镍

采用硝酸、高氯酸消解大气颗粒物样品,以丁二酮肟显色,正丁醇萃取分离,分光光度法测定大气颗粒物中镍的含量。线性回归方程为A=0.2056c-8.027×10~(-3),相关系数r=0.9994,线性范围为0.01～2.44 mg/L,回收率为96％～105％,RSD为0.2％～1.5％,以3倍信噪比计算,镍的检出限为7.5×10~(-3)mg/L。     

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.