分析化学创新设计性实验——基于响应面法优化中药挥发油提取工艺研究*

将响应面法与中草药挥发油提取研究有机融合并考察其抗氧化性能的创新设计性实验面向中药特色专业开设。通过考察料液比、浸泡时间和提取时间等工艺条件,让学生掌握分析化学、无机化学中的提取理论知识。通过对不同工艺条件的响应面分析,让学生掌握响应面优化法的原理及操作步骤。通过对挥发油抗氧化性能的研究,让学生掌握仪器分析中紫外分光光度计的使用。     

地锦草有效成分的提取及其生物活性的研究

采用乙醇浸提法来提取地锦草中的有效成分,并对其生物活性进行研究。探讨了地锦草总黄酮的最佳提取工艺;通过体外抗氧化实验,对地锦草提取物的抗氧化活性进行研究;同时考察了提取物对大肠杆菌、枯草芽孢杆菌、青霉、曲霉的抗菌性能,并对地锦草提取物对α-淀粉酶的抑制活性进行研究。实验结果表明:地锦草总黄酮最佳提取工艺为乙醇体积分数为85%,料液比为1∶15,提取次数为3次;体外抗氧化实验表明,地锦草具有抗氧化活性,且在浓度为8 mg/mL最为明显;抗菌性能实验表明,地锦草具有抗菌性能,且对青霉、曲霉的抗菌效果比较显著;α-淀粉酶的抑制活性的实验表明,地锦草提取物对α-淀粉酶的活性有抑制能力,在pH 6.8、浓度为4.8 mg/mL、温度为70℃时,其对α-淀粉酶的抑制效果达到最大。     

地锦草总黄酮最佳提取分离工艺的研究

采用四因素三水平的正交实验方法,对地锦草总黄酮的最佳提取工艺进行了探索.采用乙酸乙酯萃取、酸碱沉淀、铅盐沉淀3种方法,对其最佳分离工艺进行了探索.正交实验结果表明:温浸法中四因素对地锦草黄酮的影响顺序为乙醇浓度>样液比>提取温度>提取时间.通过实验得到了地锦草总黄酮的最佳提取工艺:以10倍体积的50%的乙醇水溶液在80℃浸提1 h.地锦草总黄酮的最佳分离方法为酸碱沉淀法.这些数据为中药地锦草的开发和应用提供了科学依据.     

鸡血藤中黄酮类化合物提取工艺的研究

对提取鸡血藤中黄酮类物质的工艺条件进行优选。在单因素考察的基础上,选用4个实验因素(提取温度、提取时间、料液比、乙醇体积分数)进行3水平正交试验优选,确定提取鸡血藤中总黄酮的最佳工艺参数。4种因素对鸡血藤中总黄酮提取结果的影响程度由大到小的次序为提取时间、乙醇体积分数、提取温度、料液比。总黄酮最佳工艺条件:料液比1∶30、乙醇体积分数50%、提取温度80℃、提取时间3 h,在此工艺条件下,鸡血藤中总黄酮的提取率为7.75%。该提取工艺合理,总黄酮提取率高。     

金银花中总黄酮的光谱分析及抗氧化性能测定

采用超声波法从金银花中提取黄酮类化合物,并建立了金银花中总黄酮的光谱分析方法。本法的回收率为98.0%～103.0%,RSD<0.62%。并用流动注射化学发光法研究了金银花的抗氧化性能,实验结果表明:金银花具有较强的抗氧化性能。     

超声波辅助提取茶叶总黄酮及抗氧化活性分析

采用超声波辅助法探讨了铁观音茶叶中总黄酮的最佳提取工艺条件,并测定了铁观音茶叶总黄酮清除羟基自由基的能力.结果表明,超声波功率400 W,料液比1∶30 g·mL~(-1),浸提时间30 min,乙醇浓度50%为超声波辅助提取铁观音茶叶总黄酮的最佳工艺条件,总黄酮提取率为4.74%;抗氧化实验表明随着铁观音茶叶总黄酮浓度的增大,其对羟基自由基的清除能力增大,当浓度达到0.80 g/L,清除率为65.14%,与BHT相比具有较强的抗氧化能力.     

棉杆木质素提取及其对聚丙烯抗氧化性能分析的综合性实验

介绍了一个以从新疆废弃棉花秸秆中提取出的木质素为原料及其对聚丙烯(PP)抗氧化性能为一体,针对高分子相关专业开设的综合性实验。基于新疆大学高分子相关专业的实际情况,将教师的科研项目与本科教学相结合,该综合性实验主要包括了棉杆木质素的提取、人工加速老化试验和抗氧化性能表征分析的特色实验体系。在实践教学中,学生不仅学习了棉杆木质素的提取过程,还认识了人工加速老化试验对材料的老化机理及其对抗氧化性能的影响,也拓宽了对专业知识的综合理解,为科研成果转化为教学实验提供了借鉴。     

基于多指标评价法的蒲公英提取工艺优化

以超声提取法提取蒲公英有效成分，选择总黄酮、咖啡酸、绿原酸和菊苣酸为评价指标，结合AHP-CRITIC法计算各指标权重；在单因素试验的基础上，利用Box-Behnken法优化蒲公英超声提取工艺。实验结果表明超声提取法提取蒲公英的最优提取工艺参数为：液料比5∶1,甲醇浓度60%,提取时间26 min,在此工艺条件下预测综合评分为73.26,验证实验所得综合评分为74.13±2.63,RSD为3.55%。本研究优化的蒲公英超声提取工艺适合于蒲公英中总黄酮、咖啡酸、绿原酸和菊苣酸的提取，其工艺稳定、可靠，可为蒲公英资源的开发和利用提供参考。     

竹叶提取物的抗氧化活性研究

一般认为黄酮是竹叶提取物中抗氧化作用的有效成分,黄酮含量越高,抗氧化能力越强[1-3]。本实验对不同溶媒竹叶提取物的抗氧化能力做了比较研究,发现抗氧化作用与黄酮含量并不完全成正比关系;并通过进一步的定性实验,证明黄酮并不是竹叶提取物中的唯一的抗氧化有效成分,还有其它     

竹叶提取物对铝在HCl溶液中的缓蚀作用(英文)

用不同浓度的C2H5OH(体积分数:20%-80%)从金竹竹叶中提取制备出竹叶缓蚀剂(简称为PSLE),用紫外-可见(UV-Vis)光谱和傅里叶变换红外(FTIR)光谱对其进行了表征,并对总黄酮含量进行了测定.采用失重法、动电位极化曲线、电化学阻抗谱(EIS)和扫描电子显微镜(SEM)研究PSLE在HCl介质中对铝的缓蚀作用.采用量子化学密度泛函理论(DFT)研究了两个主要竹叶黄酮成分牡荆苷和异牡荆苷的吸附方式.结果表明:PSLE对铝具有良好的缓蚀作用,且在铝表面的吸附符合Langmuir吸附等温式.缓蚀率随其浓度的增加而增大,但随温度的升高和盐酸浓度的增加而降低.竹叶总黄酮含量和竹叶缓蚀剂的缓蚀性能有良好的相关性,初步推测竹叶缓蚀剂的有效成分主要为竹叶黄酮类化合物.PSLE为阴极抑制型缓蚀剂;EIS在高频区呈容抗弧,在低频区呈感抗弧,添加PSLE后,阻抗值显著增大.SEM表明添加PSLE对铝的腐蚀产生了明显的抑制作用.量子化学计算结果表明,牡荆苷和异牡荆苷的吸附中心主要集中在竹叶黄酮骨架(FBS).     

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.