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%。     

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%.     

响应面法优化微波提取翻白草总黄酮

利用响应面法研究了翻白草总黄酮的微波辅助提取工艺.在单因素试验的基础上,以乙醇体积分数、液固比、提取温度、微波时间为自变量,总黄酮的得率为响应值,研究各因素及其交互作用对黄酮得率的影响.结果表明其最佳提取条件是:乙醇体积分数55%、液固比32 m L/g、温度82℃、微波时间10 min.此条件下,翻白草中黄酮的提取率为6.96 mg/g,与理论预测值基本吻合.     

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。     

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%.     

杨梅素的提取工艺研究

对杨梅树叶中杨梅素的提取有影响的有机溶剂浓度、提取温度、料液比、提取时间进行正交优化。结果表明,最佳提取工艺条件是乙醇体积分数95％,提取温度95℃,提取时间1．5h,料液比1：15,在此工艺条件下杨梅素提取率达到0．088％。     

何首乌中蒽醌类物质的超声波提取工艺优化

采用超声波辅助法提取何首乌中蒽醌类物质.讨论了甲醇体积分数、提取时间、提取温度、料液比和提取功率5个因素对提取效率的影响;通过正交试验确定了何首乌中蒽醌类物质的最佳提取工艺条件,甲醇体积分数为80%,提取时间为1.0h,提取温度为45℃,料液比为1∶15(g∶mL),提取功率为700W.此条件下蒽醌类物质的最大提取率为1.472 9%.     

藜蒿中黄酮类化合物的微波辅助萃取研究

应用密闭微波萃取装置,分别对藜蒿茎和藜蒿叶中黄酮类化合物进行微波萃取研究。采用正交试验方法得到微波提取藜蒿中黄酮类化合物的最佳条件。微波提取藜蒿茎的最佳条件为乙醇体积分数70％,微波功率800W,提取温度80℃和料液比1：20;微波提取藜蒿叶的最佳条件为乙醇体积分数70％,微波功率600W,照射时间12min,提取温度70℃和料液比1：20;在最佳条件下,藜蒿茎和叶中总黄酮提取率分别为6．43％和7．01％。并将微波萃取与乙醇回流提取进行了比较。     

川佛手中多酚类物质的微波和超声波联合提取工艺优化

采用微波和超声波提取技术,实现了川佛手中多酚类物质的有效提取.在微波功率800 W和微波提取时间40 min的条件下,通过单因素实验条件优化,考察了超声功率、乙醇浓度、提取温度、超声时间和提取料液比对提取效率的影响;通过正交试验设计,确定了最佳提取工艺条件参数,即超声功率800 W、乙醇体积分数60%、提取温度55℃、超声时间1.0 h和提取料液比1∶20 g/m L;通过验证实验,得到川佛手多酚的提取率约为20.79 mg/g.     

大叶榕须有效成分提取工艺研究

本文对大叶榕榕树须的黄酮类化合物有效成分进行了提取,并利用分光光度法对黄酮类化合物进行了测定。以芦丁绘制标准曲线得出回归方程为:A=12.191C(mg.m-l1)-0.0016,r=0.9996。通过溶剂筛选实验,确定乙醇较适合大叶榕须中黄酮类化合物的提取。确定了乙醇加热回流提取的最佳工艺条件为:乙醇浓度70%,提取温度70℃,料液比1∶15,提取时间2.5h。在此工艺条件下提取,大叶榕榕须总黄酮的提取率为3.71%。正交试验结果表明,影响大叶榕须总黄酮提取率的因素的主次顺序为:提取次数料液比提取时间乙醇浓度。     

利用手持技术改进测定乙醇分子结构实验

利用压强传感器代替排水集气法,改进测定乙醇分子结构实验的仪器装置,并探索最佳反应条件。另外,设计两个空白实验,结合压强变化曲线对实验误差进行相关讨论。     

Neutral diterpenoids of oleoresins of five species of conifers of Transcarpathia

The compositions of the neutral diterpenoids of the oleoresins of five species of conifers growing in the Transcarpathia have been studied. It has been found that the oleoresins ofAbies alba M.,Larix decidua M., andPicea excelsa L. contain more than 50% of neutral diterpenoids. The group and qualitative compositions of the oxygen-containing diterpenoids have been determined. In the oleoresins ofAbies alba,Picea excelsa, andPicea abies tertiary alcohols — cis-abienol and isocembrol — predominate, while inLarix decidua the main component is the hydroxy ester larixyl acetate. Primary alcohols related to the resin acids have been found in all the oleoresins investigated. Features of the distribution of diterpenoids according to the species of conifers have been revealed. The results obtained are necessary for the chemotaxonomy of conifers of the family Pinceae.Novosibirsk Institute of Organic Chemistry, Siberian Branch, Academy of Sciences of the USSR. Translated from Khimiya Prirodynkh Soedinenii, No. 6, pp. 812–816, November–December, 1988.     

光谱仪测试范围的扩展

由于石化行业的生产需要，其材质的使用具有多样性和广泛性，经常会出现顾客委托的测试样品的一个或几个元素跨越光谱仪现有测试程序测量范围的情况。本法通过对光谱仪测试原理的认识，根据光谱仪的测试能力及标样的采集，实现了一个或几个元素测量范围的扩展，并对其测量的影响因素进行了研究。     

Dichroism of absorption and polarization of phosphorescence of molecules of the closed form of nitrobenzospirothiopyran

The spectral-polarization characteristics of absorption and phosphorescence of molecules of the initial form of nitro-substituted indolinospirobenzothiopyran were studied in oriented polyethylene films and in solutions with different polarity. An oscillator model of the electron transitions responsible for the formation of absorption and luminescence spectra was suggested. It was established that the principal differences in the spectral and photophysical properties of the compound studied and its oxygen-containing analog are associated with the fact that the electronegativity of the S atom is lower than that of the O atom. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 6, pp. 1143–1146, June, 1997.     

Influence of viscosity of medium on processes of oxygen quenching of excited states of mesoporphyrin

The oxygen quenching rate constants for singlet and triplet excited states of the dimethyl ester of mesoporphyrin IX increase with decreasing viscosity of the medium and reach a maximum at a viscosity of approximately 0.4 mPa·sec, after which the rate constants begin to decrease. The drop in rate constant with increasing fluidity of the medium may be related to a nonequilibrium character of the elementary act in the interaction of the reactants in the solvent cage. In viscous media such as isopropyl alcohol, isobutyl alcohol, and isoamyl alcohol, the reaction radius is greater than the sum of the radii of the reacting particles. The long-range character of these processes is due to the relatively weak dependence of the quenching probability on distance.Translated from Teoreticheskaya i Éksperimental'naya Khimiya, Vol. 25, No. 2, pp. 161–167, March–April, 1989.     

Determination of heats of detonation and influence of components of composite explosives on heats of detonation of high explosives

The heats of detonation of 20 simple high explosives and explosive mixtures were determined by means of an adiabatic detonation calorimeter designed by the authors. The results indicated that the performance of the instrument was reliable and the experimental data were very accurate. For explosive mixtures, there was a linear accumulative relationship between the heats of detonation of the explosive mixture and its components. Accordingly, the heats of detonation of explosive mixtures could be calculated directly from the heats of detonation of simple explosives and the characteristic heats of other components. The experiments showed that the gold or brass shell of the cylindrical charge could be substituted by a thick-walled porcelain shell, which had the advantage of cheapness.

     

物质分配系数的测定实验改进

实验教学目的是从解决实际问题出发,以实验技术训练和实验设计思想培养为目标。介绍了将单一的物质分配系数测定实验改进为综合实验,提高了实验效果及实验资源利用率。     

Calculation of enthalpies of hydrogenation of hydrocarbons

Sets of hydrogen molecule equivalents have been developed which permit the calculation of hydrogenation of different types of carbon-carbon bonds from ab initio total energies (3-21G and 6-31G* basis sets, and, to a more limited extent, for MP2/6-31G* data) of reactants and products. The calculated enthalpies of hydrogenation are in good agreement with experiment for unstrained molecules, with average errors on the order of 2 kcal/mol. The 6-31G* equivalents allow the enthalpies for strained molecules to be calculated accurately, but the 3-21G equivalents do not. The equivalents for both basis sets have been tested by calculating the enthalpies of hydrogenation of carbon-carbon bonds in nitrogen- and oxygen-containing organic molecules, free radicals, and classical carbocations. The results are in good agreement with experiment in most cases.     

非那雄胺合成工艺改进

非那雄胺能抑制5α-还原酶的活性,明显降低二氢睾酮水平,是一种治疗良性前列腺增生的有效药品。该合成工艺以甾烯酮酸为原料,将其与氯化亚砜反应,无须分离即与叔丁胺反应得17β-酰胺化合物,再氧化开环,环合,氢化,脱氢合成了非那雄胺。经元素分析、IR、1HNMR、13CNMR、MS分析表征了其结构。该法无须使用昂贵的2,2-二吡啶二硫化物和剧毒药品苯亚硒酸酐,且以乙酸铵代替氨气,降低了对设备的要求和腐蚀,更适用于工业生产。