微波辅助条件下鱼腥草中癸酰乙醛的高效提取

以乙酸乙酯为溶剂,在微波辅助条件下提取鱼腥草挥发油,考察了微波温度、功率及时间对鱼腥草挥发油提取率及鱼腥草素(癸酰乙醛)含量的影响,探讨了鱼腥草挥发油储存过程中癸酰乙醛的化学转化。研究发现,在温度80℃、功率1 000 W及时间12min的微波辅助条件下,鱼腥草挥发油的提取率高达0.66%,挥发油中癸酰乙醛的含量高达60.78%。在微波辅助条件下,较低的提取温度及快速提取有效避免了癸酰乙醛的氧化分解是其高效提取的根本原因,鱼腥草挥发油中存在癸酰乙醛与其二聚物的动态平衡是癸酰乙醛长时间保持稳定的主要原因。     

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。     

万寿菊不同部位挥发性化学成分比较研究

通过分析不同部位万寿菊挥发性化学成分,为万寿菊的开发利用提供实验依据.采用同时蒸馏.萃取法(SDE)提取不同部位万寿菊挥发油,气相色谱法分离,质谱法鉴定结构.结果表明万寿菊花、叶、茎挥发油的含量分别为3.7%、3.5%和2.9%.在花、叶和茎挥发油中分别鉴定出40、33和35种化学成分.万寿菊不同部位挥发油的含量及其化学成分存在一定的差异,其中万寿菊花挥发油的含量最高,万寿菊花、叶、茎挥发油中柠檬烯、3,7-二甲基-1,6-辛二烯.3-醇、1-环己基-2.甲基-丙烯-2-酮和3-甲基-6-(1-甲乙基)-2-环己烯-1-酮含量较高.     

溶剂浸提条件下鱼腥草中癸酰乙醛的高效提取

本文采用溶剂浸泡提取鱼腥草挥发油,考察了浸泡溶剂、浸泡温度和浸泡时间等因素的影响,探究了鱼腥草中最关键的抗菌成分之一鱼腥草素(癸酰乙醛)的真实含量。研究发现,室温下采用乙酸乙酯浸泡鱼腥草456h,鱼腥草挥发油的提取率高达0.294%,挥发油中癸酰乙醛的含量高达40.14%,仅检测到少量甲基正壬酮。结果表明,温和的提取条件有效抑制了癸酰乙醛的氧化分解,获得远高于水蒸汽蒸馏条件下的癸酰乙醛含量(0.03%)。该研究为从鱼腥草中高效提取癸酰乙醛提供了一种切实可行的手段。     

减压提取与常压提取柴胡挥发油品质比较

对比减压和常压条件下提取的柴胡挥发油在成分、含量及药效方面的差异,考察挥发油的品质,优选提取方法.采用气相色谱-质谱联用(GC-MS)法分析柴胡挥发油成分及其相对含量,再采用气相色谱法建立挥发油中己醛、庚醛、正辛醛和反式-2,4-癸二烯醛的含量检测方法,测定不同压力下提取的柴胡挥发油有效成分含量,通过背部皮下注射酵母混...     

超临界流体萃取-GC-MS分析西黄丸中挥发性成分

建立西黄丸中挥发油成分乙酸辛酯的含量测定方法,为西黄丸的质控标准提供依据。方法:超临界CO2萃取西黄丸中挥发油成分,采用气相色谱法测定乙酸辛酯含量;研究压力、温度、时间和粒度因素对挥发油得率与乙酸辛酯含量的影响,并进行了化学计量学分析。采用GC-MS分析了适宜条件的挥发油的成分。综合考虑挥发油得率和乙酸辛酯含量双指标,确定的西黄丸挥发油萃取条件为:粉碎粒度为80目,萃取压力为25 MPa,温度为40℃,时间为2 h。在此条件下,挥发油得率达到7.76%,乙酸辛酯含量达到0.72 mg·g^-1。通过指纹图谱、主成分分析(PCA)、正交偏最小二乘判别分析(OPLS-DA)化学计量学分析可知,不同萃取条件对所提取的挥发油物质组分及其含量没有显著性差异。GC-MS鉴定出的主要成分有(1S-endo)-2-甲基-3-亚甲基-2-(4-甲基-3--3-戊烯基)-二环[2.2.1庚烷、10α-羟基日本刺参萜、(±)-麝香酮、4-亚甲基-2,8,8-三甲基-2-乙烯基-双环[5.2.0]壬烷和2-甲基-4-(2,6,6-三甲基-1-环己烯-1-基)丁醛。结论:西黄丸挥发油成分适宜萃取条件,及建立的乙酸辛酯含量测定方法准确、可靠,为有效控制西黄丸质量,完善其质量标准及进一步的药效成分研究提供了科学依据。     

微波辅助提取GC-MS分析莪术挥发油成分

1引言 莪术是我国传统中药材,是一种有效的抗癌中药,在防治恶性肿瘤特别是早期宫颈癌方面有较好的疗效.据<本草纲目>记载:莪术辛、苦、温,归肝、脾经,具有行气破血、消积止痛之功效,被称为血中之气药.莪术根茎中含挥发油约1%～2.5%,为多种倍半萜类,其中莪术醇和榄香烯以及莪术酮和莪术二酮具有抗肿瘤、抗病毒的疗效.微波辅助提取具有设备简单、适用范围广、萃取效率高、节省时间和溶剂、污染小等诸多优点,应用范围已从最初的环境样品分析迅速扩展到食品、化工和农业等领域.本研究以莪术为原料,采用微波萃取法提取挥发油,通过紫外分光光度法监测其含量变化,用气相色谱-质谱法(GC-MS)分析最优提取工艺条件下所得挥发油成分,为进一步开发莪术药用价值提供依据.     

山苍子雄花和雌花挥发油的提取及成分分析

山苍子的根、叶和果实中均含有精油,山苍子油的主要成分为柠檬醛。采用水蒸汽蒸馏法提取山苍子花挥发油,对雄花和雌花分别提取。并利用GC-MS气质联用仪对两组挥发油进行分析检测,确定其化学成分及相对百分含量。从雄花挥发油中鉴定出43种成分(占挥发油总含量的88.15%),从雌花挥发油中鉴定出30种成分(占挥发油总量的85.53%)。     

苦碟子挥发油化学成分的分析

对我国东北地产苦碟子中挥发油成分进行系统分析,确定挥发油的化学成分,为阐述其生物活性提供依据.采用水蒸汽蒸馏法提取挥发油,气相色谱--质谱联用仪进行分析.结果鉴定出37种化合物.在这些化合物中,脂肪烷烃类占53.21%,酮、醛类占39.05%,烯、烯醇、烯酸类占4.94%,酯类占1.57%.其挥发油的主要成分是6,10,14-三甲基-2-十五烷酮,含量为33.98%.     

气相色谱-质谱联用法测定黄兰中挥发油化学成分

采用水蒸气蒸馏法、超临界萃取法、微波辅助提取法与超声波辅助萃取法等4种提取方法提取黄兰挥发油,运用毛细管气相色谱-质谱联用法结合计算机检索对其挥发油化学成分作了鉴定和测定.结果显示从水蒸气蒸馏法、超临界萃取法、微波辅助提取法与超声波辅助萃取法所得挥发油中分别鉴定出了36,35,25和26种化合物.用面积归一法测定了4种挥发油中各种化学成分的相对百分含量,各占总峰面积的92.62%,91.46%,93.18%和95.53%.虽然不同提取方法所得的4种挥发油化学成分有所不同,但其中有20种化合物包括β-荜澄茄烯、大根香叶烯D、丁香烯氧化物、丁香烯等为4种挥发油提取物所共有.     

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。     

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。     

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。