葵花籽粕蛋白质、绿原酸分步提取工艺参数优化

在单因素试验的基础上,选取NaCl浓度、提取温度、料液比为自变量,以蛋白质提取率为响应值;选取乙醇体积分数、提取时间、料液比为自变量,以绿原酸的提取率为响应值,利用响应面法对葵花籽粕蛋白质、绿原酸的提取工艺进行优化,得到回归方程的预测模型。结果表明,最佳提取工艺条件为:蛋白质NaCl浓度1.51mol/L、液料比1∶12.88(g/mL)、提取温度60.27℃;绿原酸乙醇体积分数56.07%、液料比1∶16.03(g/mL)、提取时间47.06min.在此条件下,葵花籽粕蛋白质和绿原酸的提取率分别为36.64%和2.73%.     

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。     

微波法提取水蓼中总黄酮的工艺研究

研究了水蓼中总黄酮的微波提取最佳工艺。采用单因素试验和正交试验考察微波功率、乙醇浓度、微波辐射时间、料液比对水蓼中总黄酮提取率的影响,优选提取工艺。最佳工艺条件为:微波功率为520W,乙醇浓度为60%,微波辐射60s,间歇辐射3次,料液比为1g∶20mL。结果表明,微波提取具有提取率高、提取速度快等特点,用于中草药的提取应用前景广阔。     

响应面法优化红枣中硒的提取工艺及HPLC测定

探讨研究红枣中微量硒的提取工艺。采用响应面法中的Box-Behnken试验设计原理选取试验因素与水平,对红枣中硒的提取率有影响的料液比、消化液配比和消化时间3个因素进行优化.试验结果表明:硒的最佳提取工艺参数料液比为1∶12.56(g/mL)、消化液配比为1∶3.6、消化时间为137.2min;在此条件下,红枣中硒的提取率为0.294μg/g.该研究为从食品中提取检测微量硒提供了可行的手段.具有一定的实用价值.     

正交试验与响应面法优化微波提取地黄多糖工艺研究（英文）

为了获得微波提取地黄多糖的最佳条件,采用正交试验法和响应面法分别优化微波提取地黄多糖工艺,以地黄多糖得率为指标,采用微波提取地黄多糖,苯酚-硫酸法测定地黄多糖的含量,以微波提取时间、提取温度和料液比进行三因素分析,根据单因素试验结果设计正交试验和响应面试验,进一步优化微波提取地黄多糖工艺。微波提取地黄多糖工艺通过正交试验法优化的结果表明,最佳条件为微波提取时间150 s,提取温度80℃,料液比1 g∶10 mL,该条件下的地黄多糖得率为72.10%。响应面法优化微波提取地黄多糖工艺的结果表明,修正后的最佳工艺条件为微波提取时间137 s,提取温度89℃,料液比1 g∶8 mL,该条件下的地黄多糖得率为74.41%。经过两种优化方法的比较,响应面法适合优化微波提取地黄多糖工艺,能够有效提高地黄多糖得率。     

茶叶多酚和多糖同步提取工艺优化及硒配合物的制备

以茶叶为原料,在单因素试验的基础上,利用响应面法对茶叶多酚、多糖的提取工艺进行优化;得到回归方程的预测模型。实验结果表明,最佳提取条件为茶多酚:料液比1∶53.75 g·mL~(-1)、超声时间50.00 min、乙酸乙酯33.60 mL,在此条件下茶多酚的提取率8.47%;茶多糖:料液比1∶58.42 g·mL~(-1)、超声时间41.71 min、乙酸乙酯40.00 mL,在此条件下茶多糖的提取率4.93%。采用红外光谱对茶多酚、茶多糖与Se相结合形成的配合物进行结构表征。     

景天三七总多酚提取工艺的优化及活性研究

采用超声提取景天三七中的多酚,并利用Box-Behnken响应面法对影响景天三七总多酚提取率的因素(液料比、乙醇浓度、超声时间、超声温度)进行了优化,并以DPPH自由基和ABTS自由基清除能力为评价指标,研究景天三七总多酚体外抗氧化活性。结果显示,最佳的提取条件为乙醇浓度63%,液料比36∶1(mL·g~(-1)),超声温度65℃,超声时间27 min。此条件下多酚的提取率为(28.08±0.21)mg·g~(-1)。此条件下得到的景天三七总多酚对DPPH自由基和ABTS自由基具有不同的清除能力,其半数抑制浓度(IC_(50))分别为0.81μg·mL~(-1),9.02μg·mL~(-1)。本研究为景天三七的资源开发提供理论基础。     

正交试验结合响应面法优化诃子多糖提取工艺

采用正交试验结合响应面法优化诃子多糖的提取工艺,以诃子多糖的提取率为指标,以固液比、提取温度、提取时间和提取次数为因素,正交试验初步筛选工艺参数,响应面法做进一步优化.结果表明,多糖提取的最佳工艺条件为固液比1∶28,提取温度69℃,提取时间1h,提取次数3次,各项指标相对误差均小于2%,应用响应面法可减少诃子多糖提取时间.     

超声波法提取紫甘薯叶总黄酮的工艺研究

采用超声波提取法,以总黄酮含量为考察指标,利用单因素试验法对影响总黄酮提取率的因素进行了分析,然后通过正交试验确定紫甘薯叶总黄酮的最佳工艺条件。研究表明,影响紫甘薯叶总黄酮提取率的主次因素为:溶剂pH值溶剂的浓度料液比提取时间。紫甘薯叶总黄酮的最佳提取工艺为:乙醇体积分数80%,料液比1∶40(W/V),提取时间30 min,提取溶剂pH 9。在此条件下甘薯叶中总黄酮提取率为8.22%。     

超声波提取川贝母黄酮类物质的工艺优化

采用超声波提取技术提取川贝母中的黄酮类物质.考察了超声功率、乙醇体积分数、料液比、超声时间和超声温度各因素对黄酮类物质提取效率的影响.在超声功率800 W条件下,通过L_9(3~4)正交试验,确定了川贝母黄酮类物质的超声波最佳提取工艺参数:超声功率为800 W,乙醇体积分数为80%,料液比为1 g∶45 mL,超声时间为2.0 h,超声温度为45℃.在最佳提取工艺条件下进行验证试验,川贝母黄酮类物质的提取率达到77.13 mg/g,RSD值为0.39%.     

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.