HPLC法同时测定忍冬叶中9种活性成分的研究

为了有效利用忍冬植株,建立了同时检测忍冬叶中新绿原酸、绿原酸、咖啡酸、芦丁、木犀草苷、金丝桃苷、异绿原酸C、木犀草素和槲皮素9种活性成分含量的HPLC分析方法,并用于忍冬叶中活性成分的定量测定,为忍冬叶多指标质量评价标准提供理论依据和方法参考.     

高效液相色谱法同时测定忍冬中7种成分

建立了在不同时间段内转换使用不同波长同时测定忍冬花和叶中7种化学成分(绿原酸、咖啡酸、芦丁、木犀草苷、异绿原酸A、异绿原酸B、异绿原酸C)的高效液相色谱分析方法,同时应用该方法分析了忍冬花、忍冬老叶和新叶中成分含量的差异。色谱柱为Agilent Eclipse Plus C18(250 mm×4.6 mm, 5 μm);流动相为0.3%甲酸水溶液(A)和乙腈(B),梯度洗脱,流速1 mL/min;采用VWD紫外检测器转换波长(330 nm、350 nm)检测。应用所建立的方法测定忍冬新叶中绿原酸、木犀草苷含量分别为2.572%、1.498‰,均比药典中规定的含量高,有必要进一步的研究和开发利用。该方法准确、简便、灵敏度高,适用于忍冬中7种化学成分含量的同时测定和忍冬的质量控制及综合评价。     

栽培宽叶羌活中有机酸和香豆素含量的季节动态变化研究

采用高效液相色谱-二极管阵列检测法(HPLC-DAD)测定2、3年生不同月份(5月、6月、7月、8月和9月)采集的栽培宽叶羌活中绿原酸、阿魏酸、紫花前胡苷、补骨脂素、佛手柑内酯、欧前胡素、羌活醇和异欧前胡素的含量,考察采收时间和生长年限对栽培宽叶羌活主要活性成分含量的影响。结果表明,2、3年生栽培宽叶羌活各活性成分在返青及生长初期(5~6月份)含量较高,在生长旺盛的花果期(6~7月份)呈明显下降趋势,8月份达到最低水平,9月份又略有回升。2年生栽培宽叶羌活所测活性成分总含量在不同月份均低于3年生栽培宽叶羌活。生长年限和采收时间对宽叶羌活活性成分含量的积累具有重要影响,本研究对于宽叶羌活的进一步研究和开发应用提供了科学依据。     

闪式提取HPLC-DAD测定金银花中绿原酸和木犀草苷

采用闪式提取法和超声提取法分别提取金银花及其叶中的绿原酸和木犀草苷,建立HPLC-DAD分析方法进行评价,为金银花药材及相关产品的快速质量控制探索新方法。采用乙腈-1%甲酸水溶液体系经梯度洗脱,在AgilentC18色谱柱上实现了绿原酸和木犀草苷的同时基线分离,绿原酸在3.96~253.2μg/mL(326 nm,R=0.9998)、木犀草苷在0.53~34μg/mL(350 nm,R=0.9997)范围内具有良好的线性关系,方法具有良好的精密度和回收率。闪式提取3 min,金银花及其叶中绿原酸和木犀草苷的提取率均略高于超声提取法(超声3次×45 min,浸泡16 h)。组织破碎闪式提取法为金银花药材中绿原酸和木樨草苷的快速提取及质量控制提供了一种新方法。     

金银花不同部位中绿原酸和木犀草苷含量的测定

利用HPLC法测定金银花不同部位中绿原酸和木犀草苷。采用ODS-C18色谱柱(250 mm×4.6 mm,5μm),以甲醇-水(0.03 mol/L磷酸)为流动相进行梯度洗脱,流速:1.0 mL/min,检测波长:350 nm,柱温:室温。绿原酸浓度在0~0.4 mg/mL内与峰面积呈良好线性关系(r2=0.999 6),回收率为101.9%~105.2%,相对标准偏差为3.18%(n=6)。木犀草苷浓度在0~0.1 mg/mL内与峰面积呈良好线性关系(r2=0.999 1),平均回收率为100.5%~104.0%,相对标准偏差为3.42%(n=6)。结果表明:金银花、芽等部位绿原酸和木犀草苷的含量较高。     

HPLC法同时测定24种花中的5种活性成分含量

建立了高效液相色谱法(HPLC)同时测定24种花中绿原酸、金丝桃苷、槲皮素、木犀草素和异鼠李素含量的方法。采用C18柱(250 mm×4.6 mm,5μm),流动相为甲醇-0.2%冰乙酸溶液梯度洗脱,检测波长350 nm,柱温35℃,流速0.8 mL/min。绿原酸、金丝桃苷、槲皮素、木犀草素和异鼠李素分别在0.0208~104.00μg/mL(r=0.99993),0.017~85.00μg/mL(r=0.99998),0.0172~86.00μg/mL(r=0.99997),0.0304~152.00μg/mL(r=0.99997),0.0168~84.00μg/mL(r=0.99986)范围内与峰面积呈良好的线性关系,平均加标回收率(n=9)92.26%~99.09%,仪器精密度(n=6)RSD均小于3.1%,方法重复性(n=6)的RSD均小于3.6%。方法可同时测定这24种花中绿原酸和黄酮类物质的含量,可作为花中活性成分定量分析的方法。     

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.     

高效液相色谱法测定野生和人工种植库鲁木提草中柚皮苷和木犀草素的含量

本文建立了新疆库鲁木提草中柚皮苷和木犀草素两种活性成分的高效液相色谱同时测定方法,并实现了野生及人工栽培库鲁木提草中柚皮苷和木犀草素的检测。采用Agilent HC-C_(18)色谱柱(250×4.6mm,5μm)分离,以甲醇-0.2%HAc水溶液作为流动相,在柱温为室温和流速1.00mL/min条件下进行梯度洗脱,实现了两种活性成分之间以及它们与干扰组分的良好分离。柚皮苷和木犀草素的线性范围分别为120~1 440mg/L(r=0.9998)和17.5~210mg/L(r=0.9999),加标回收率分别为93.8%~100.2%(RSD=1.8%~2.7%,n=3)和98.3%~100.6%(RSD=1.3%~2.9%,n=3)。研究结果表明野生库鲁木提草中柚皮苷和木犀草素的含量更高。     

高效液相色谱–波长切换法同时测定独一味软胶囊中6种成分

建立高效液相色谱–波长切换法同时测定独一味软胶囊中山栀苷甲酯、绿原酸、8-O-乙酰山栀苷甲酯、连翘酯苷B、毛蕊花糖苷和木犀草苷的方法。以Symmetry Shield RP18柱(250 mm×4.6 mm,5 μm)为色谱柱,乙腈–0.3%磷酸水为流动相,检测波长分别为235 nm(山栀苷甲酯、8-O-乙酰山栀苷甲酯)、330 nm(绿原酸、连翘酯苷B、毛蕊花糖苷)、360 nm(木犀草苷),流量为1 mL/min。山栀苷甲酯、绿原酸、8-O-乙酰山栀苷甲酯、连翘酯苷B、毛蕊花糖苷和木犀草苷的进样量在各自的范围内与色谱峰面积线性关系良好,相关系数不小于0.999 0,测定结果的相对标准偏差为0.21%～0.69%(n=6),平均加标回收率为94.0%～101.1%。该方法简单、准确、重现性好,适用于独一味软胶囊的质量评价。     

ZIF-8吸附材料对雪菊中木犀草苷的富集及在微型近红外光谱分析中的应用EI北大核心CSCD

制备了SiO;@ZIF-8吸附剂并用于吸附雪菊中微量的木犀草苷,建立了基于特征变量筛选的微型近红外光谱分析方法。以木犀草苷为对象,研究了吸附剂的质量、pH、振荡时间对吸附效果的影响;在最佳条件下对富集了木犀草苷的吸附剂直接进行检测,探讨分别采用竞争自适应加权采样算法(CARS)、蒙特卡罗-无信息变量消除法(MC-UVE)和随机青蛙算法(RT)进行变量筛选,并用偏最小二乘法建立定量校正模型。研究发现,当吸附剂质量为0.20 g, pH 7时振荡20 min,木犀草苷吸附率可达到92%;经3种变量筛选后最优模型为CARS,CWT方法光谱预处理后,木犀草苷校正模型参考浓度和预测浓度两者之间的相关系数达到最佳的0.9700,预测回收率在85%~120%。SiO_(2)@ZIF-8吸附剂可以有效的富集雪菊中的木犀草苷,在CARS变量筛选下,通过微型近红外光谱可以实现雪菊中微量木犀草苷的测定。     

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。     

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。     

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.     

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.     

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。     

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.     

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。