青蒿挥发油化学成分的分析测定

青蒿[1]Artemisia annua L.又名香蒿,为菊科植物青蒿或黄花蒿的全草.分布辽宁、河北、山东、山西、江苏、广东等地.青蒿在我国各地均有大量野生,资源丰富,本植物的根(青蒿根),果实(青蒿籽)均可供药用,青蒿具有抗疟、抗血吸虫、解热、镇痛及退虚热、和胃止痛等功效.青蒿的主要成分有苦味质、挥发油和青蒿碱、维生素A等.为探讨其挥发油的成分,我们对青蒿全草进行挥发油的提取,并用GC-MS进行测定分析,从中鉴定出44个化合物.     

南鹤虱挥发油化学成分的气相色谱/质谱分析

1 引 言南鹤虱为伞形科植物野胡萝卜(Daucus carota L.)的干燥成熟果实。主产于江苏、安徽、浙江、湖北等省。南鹤虱具有杀虫消积之功效。用于治疗蛔虫、蛲虫、绦虫病，以及虫积腹痛，小儿疳积。有关南鹤虱的挥发性成分虽已有文献报道，但由于产地、环境条件的差异，不同产地的南鹤虱成分有着明显的差异。本文采用湖北省竹山县所产南鹤虱，以水蒸气蒸馏法提取挥发油（收油率为3.8%），经无水硫酸钠干燥后，进行毛细管气相色谱分析，共分离出31个峰，以归一化法计算了各个峰的相对含量，用气相色谱质谱法从中共鉴定了26个成分，占挥发油总…     

茵陈挥发油GC-MS指纹图谱分析

建立了茵陈挥发油GC-MS指纹图谱,将正交投影算法用于不同样本中共有峰的提取,提高了共有峰的识别能力,降低了由于保留时间的漂移、质谱检索匹配度不高以及色谱峰重叠而引起的共有峰识别的难度.采用共有峰率、变异率及相似度等几个指标对4个不同产地的茵陈挥发油成分进行了评价,从共性、差异和整体性等多个方面全面表征茵陈挥发油的化学模式特征.结果表明,不同产地的茵陈挥发油成分大致相同,该指纹图谱可用于茵陈中挥发油成分的质量控制.     

朱砂玉兰及其变种辛夷挥发油的化学成分比较分析

为了了解不同品种辛夷挥发油的化学成分的差异,用水蒸气蒸馏法提取了朱砂玉兰及其两个变种的辛夷挥发油,并对其化学成分进行了GS/MS分析.从三种淡黄色芳香性的挥发油中共检测出44种组分,其中朱砂玉兰的成分较为简单,主要药物活性成分桉油精(17.72%)和香料成分(58.26%)的含量均较高;萼朱砂玉兰的桉油精含量较低,但香料成分(62.66%)的含量较高;而红运朱砂玉兰的桉油精含量最高,并含有较多的特有成分.朱砂玉兰不同品种的辛夷挥发油的化学组成及化合物的百分含量存有较大差异,但均含有多种药用或香料成分,具有开发利用价值;而朱砂玉兰及其变种的辛夷挥发油自身特有的化学组成,也可为玉兰属植物的化学分类研究提供有用的信息.     

姜科姜黄属植物有效成分的研究

研究不同产地姜科姜黄属植物挥发油的化学成分,了解不同产地姜科姜黄属植物挥发性成分的差别,为控制其药材质量提供理论依据。采用水蒸气蒸馏法提取不同产地姜科姜黄属植物的挥发油,用气相色谱—质谱联用仪对其进行分离测定,结合计算机检索对分离的化合物进行结构鉴定,应用色谱峰面积归一化法测定各成分的相对百分含量。结果发现,不同产地姜科姜黄属植物的水蒸气蒸馏提取物得率在0．20％～2．13％之间,分别鉴定出24～40个化学成分。不同品种、不同产地姜科姜黄属植物的挥发油含量和其所含成分有较大差别,文献报道的某些有效成分如莪术酮、莪术二酮、莪术醇和表莪术酮在某些供试品中未检测到。实验中10个供试品药材中挥发性成分主要为单萜类及倍半萜类化合物及其衍生物,倍半萜类化合物的百分含量(44．57％～88．65％)明显高于单萜类化合物的百分含量(1．63％～26．69％)。     

微波辅助蒸汽蒸馏提取-气相色谱-质谱法测定矮化芳樟枝叶挥发油成分

采用微波辅助蒸汽蒸馏提取法对矮化芳樟枝或叶中挥发油进行提取,用气相色谱-质谱法测定其中的挥发油成分。所得结果与传统蒸汽蒸馏提取法数据对比,两种方法所得枝叶挥发油主要成分和含量基本相同;但微波辅助蒸汽蒸馏提取法仅需37.5min即可达到最高提取率。     

菌陈挥发油GC-MS指纹图谱分析

建立了菌陈挥发油GC-MS指纹图谱，将正交投影算法用于不同样本中共有峰的提取，提高了共有峰的识别能力，降低了由于保留时间的漂移、质谱检索匹配度不高以及色谱峰重叠而引起的共有峰识别的难度．采用共有峰率、变异率及相似度等几个指标对4个不同产地的菌陈挥发油成分进行了评价，从共性、差异和整体性等多个方面全面表征菌陈挥发油的化学模式特征．结果表明，不同产地的菌陈挥发油成分大致相同，该指纹图谱可用于菌陈中挥发油成分的质量控制．     

新疆藁本挥发油的抑菌活性及组分分析

为了明确中药材新疆藁本挥发油对植物病原真菌的熏蒸抑制活性及分析其化学组分,为新疆藁本挥发油在农业上的应用提供参考依据。采用水蒸气蒸馏法提取新疆藁本挥发油,通过生长速率法测定其挥发油对小麦赤霉病菌、水稻胡麻斑病菌、草莓灰霉病菌和苹果炭疽病菌4种植物病原真菌的熏蒸抑制作用,并利用气质联用仪(GC-MS)分析新疆藁本挥发油的化学组分。结果表明,新疆藁本挥发油对供试的4种植物病原真菌均有强烈的熏蒸抑制作用,有效中浓度(EC_(50))分别为0.98、1.01、1.46、2.79μL/皿。GC-MS从新疆藁本挥发油中共检测到23个组分,鉴定出其中17个,占挥发油总量的99.796%,其主要组分为肉豆蔻醚(94.328%)、2-莰烯(3.018%)等。新疆藁本挥发油可作为抑制植物病原真菌的天然活性成分资源,开发利用。     

无溶剂微波提取-气相色谱-质谱法测定八角挥发油

将干八角粉碎至过2.00mm孔径的药筛,取20g样品间歇性喷雾加水至其含水量(质量分数)达50%,置于圆底烧瓶中,用LWMC-204微波化学反应器在180W微波功率进行无溶剂微波辅助提取(SFME),所得提取液用无水硫酸钠干燥置于4℃保存。此溶液用于气相色谱-质谱法测定其中的挥发油组分,将所得结果与SFME法和水蒸气蒸馏法(SD)所得数据对比,可知SFME法提取挥发油有以下特点:①该法仅需30min提取即可达到其最高提取率7.71%;②经此法分离后在挥发油中共测得25种化合物,达总量为98.94%;③所测得的含氧单萜类化合物高于SD法提取所得;④所测得挥发油的主要成分反式茴香脑的含量较SD法提取所得的量高1.4倍。     

超临界CO2流体萃取法与水蒸气蒸馏法提取荆芥穗挥发油化学成分的研究

采用超临界CO2萃取法(SFE)与水蒸气蒸馏法(SD)从荆芥穗中提取挥发油。采用SE-54毛细管柱进行分析,用气相色谱-质谱法对挥发油中各种化学成分进行鉴定,用归一化法测定各组分的含量。色谱条件:SE-54毛细管柱 (30 m×0.25 mm i.d.,0.25 μm),柱温50 ℃(3 min)5 ℃/min180 ℃(2 min)10 ℃/min260 ℃(50 min);分流进样,分流比1∶50;进样口温度280 ℃。在采用超临界CO2萃取法提取的挥发油中共鉴定出54种成分,其主要成分为长叶薄荷酮、薄荷酮、亚油酸氯化物等;在水蒸气蒸馏法提取的挥发油中共鉴定出39种成分,其主要成分为长叶薄荷酮、薄荷酮、柠檬烯等。超临界法较水蒸气法更加稳定可靠,重现性好,适用于中药挥发油的化学成分分析。     

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。     

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.     

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。