银杏茶中总黄酮的水溶浸出行为研究

以芦丁为标准品，采用分光光度法，以Al（NO3）3-NaNO2为显色剂，测定了市售银杏茶中总黄酮的含量，并考察了银杏茶在水中浸泡时浸泡温度、浸泡时间、浸泡次数、浸泡溶液的pH值等条件对银杏茶中总黄酮浸出的影响。结果表明，银杏茶中黄酮在水中浸出量受浸泡温度和浸泡溶液DH值的影响比较大。泡茶的溶液应避免使用酸性溶液。还对银杏茶的加工工艺进行了考察研究，发现银杏叶通过微波处理后，其黄酮的浸出量明显高出烘箱烘干的银杏叶的黄酮浸出量。因此，建议在银杏茶的加工工艺中采用微波干燥处理银杏叶。     

南雄银杏叶中内酯的高效液相色谱法测定

用高效液相法分析了广东省南雄市不同采收时间，不同树龄的银杏叶中的银杏内酯含量；采用Kromasil C18柱、甲醇－水－四氢呋喃流动相、流速1mL/min、差示折光检测器、柱温35℃、外标法定量，样品用聚酰胺柱纯化，获得了满意的分离效果；结果表明银杏内酯含量随树龄不同，采收时间不同而不同，南雄银杏叶内酯平均含量为0．23％（w）。     

明日叶黄酮类化合物清除羟基自由基活性研究

为了研究明日叶黄酮类化合物对羟基自由基的清除作用,以明日叶（主要取叶片）为原料,用体积分数为65％乙醇提取明日叶总黄酮,测定其总黄酮含量.通过Fenton反应体系产生羟基自由基,利用明日叶提取液中的功能成分黄酮类化合物对羟基自由基的清除作用进行研究.结果表明：明日叶提取物总黄酮质量分数为10.18％,且黄酮类化合物对羟基自由基有较强清除效力,当提取物总黄酮浓度在0.1～1.0 mg/mL范围内,其与清除率呈正相关.明日叶中黄酮类化合物对羟基自由基有较强清除效力,作为天然抗氧化产品开发具有一定价值.     

藏药独一味药材中不同部位木犀草素和总黄酮含量的分析

测定藏药独一味药材中不同部位的木犀草素和总黄酮含量,进一步完善独一味药材的质量评价体系.分别采用高相液相色谱法和紫外分光光度法测定独一味药材的根、叶、花、全草中的木犀草素及总黄酮的含量.该方法具有很好的线性关系和回收率.独一味药材的叶、花、全草中均含有木犀草素而根中未检出;根、叶、花、全草中均含总黄酮.     

火焰原子吸收法测定九管血不同部位的微量元素

为测定九管血的不同部位Fe、Cu、Mn、Zn的含量,样品用V（HNO3）＋V（HClO4）=4＋l进行消化处理,然后在实验选定的最佳工作条件下,用火焰原子吸收光谱法（FAAS）对九管血不同部位的Fe、Cu、Mn、Zn微量元素进行测定。结果表明,九管血根、茎、叶、籽中微量元素含量丰富,其中Fe含量最高,Cu含量最低,为九管血药效的进一步研究和资源综合开发利用提供一定的科学依据。     

大孔树脂AB-8分离纯化白刺叶中的总黄酮醇苷

采用大孔树脂AB-8分离纯化白刺叶中的总黄酮醇苷,反相高效液相色谱法(RP-HPLC)对白刺叶提取物中的总黄酮醇苷进行分析。RP-HPLC法测定白刺叶提取物体积分数为70%乙醇洗脱部分,流动相:V(甲醇)∶V(0.4%H3PO4溶液)=60∶40;检测波长360 nm;结果表明,大孔树脂AB-8纯化白刺叶中的总黄酮醇苷效果良好,纯度可达到18.28%。     

不同生长期忍冬叶中活性成分的动态变化及抗菌作用研究

研究了不同生长期忍冬叶中活性成分的差异性及动态变化和抑菌活性.分别采用紫外分光光度法(UVVis)对不同生长期忍冬叶中总黄酮含量进行测定;采用气相色谱-质谱(GC-MS)联用法对不同生长期忍冬叶中的挥发性成分进行测定;采用高效液相色谱法(HPLC)对不同生长期忍冬叶中的绿原酸、新绿原酸、异绿原酸C、咖啡酸、木犀草素、木犀草苷、金丝桃苷、芦丁、槲皮素9种化合物的含量进行测定;采用平板打孔法测定不同生长期忍冬叶的抗菌活性.结果表明不同生长期忍冬叶中活性成分的含量差异较大,6月份所测各种活性成分含量均较高,且抑菌效果最好.综合不同生长期忍冬叶中各活性成分的含量,确定忍冬叶的最佳采摘期为6月份,为忍冬叶的综合开发利用提供理论依据.     

高效液相色谱法测定棉籽提取物中总黄酮醇苷的含量

建立棉子中总黄酮醇苷含量的眦测定方法.样品用V(甲醇):V(25%HCl)=4:1的混合液经90 ℃热水浴处理,采用眦法测定总黄酮醇苷含量.选用迪马-C18色谱柱,以V(甲醇):V(0.4%H3PO4)=60:40为流动相,检测波长为360nm.结果:以槲皮素、山奈素为对照品计算,棉子中总黄酮醇苷平均回收率为98.8%,RSD为2.6%.方法可用于棉子中总黄酮提取物含量的测定.     

流动注射-抑制化学发光法测定银杏叶中总黄酮含量

提出了流动注射-抑制化学发光测定银杏叶中的总黄酮含量的分析方法.它是基于银杏叶中物质黄酮类具有还原性,在碱性条件下还原H_2O_2,抑制鲁米诺-H_2O_2-KIO_4体系的化学发光,其抑制程度的大小与总黄酮的含量成线性关系.方法的线性范围为1.5～30μg/mL,检出限为0.03μg/mL,相对标准偏差(RSD)为1.2%,采样频率为240次/h,回收率为101%～104%.     

反相高效液相色谱法测定毛竹叶中总黄酮

用反相高效液相色谱法,RP－C8柱为固定相,甲醇－水－冰乙酸（40＋60＋2）为流动相,以芦丁为参照物外标法定量,辅以二极管阵列检测技术,测定了毛竹叶中总黄酮的含量,并与光度法作了比较。     

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.