气相色谱-质谱联用分析比较浙江海风藤茎及叶挥发油成分

分析比较了浙江海风藤茎及叶两个部位挥发油的化学成分.采用水蒸气蒸馏法提取,运用气相色谱-质谱联用法结合计算机检索对其化学成分进行分析和鉴定,用气相色谱面积归一法测定各组分的相对百分含量.从浙江海风藤茎及叶挥发油中分别鉴定出了30和37种化合物,其中有20种是它们共同的成分,含量最高的是喇叭茶萜醇(茎含39.62%,叶含36.80%).已鉴定挥发油成分占总挥发油含量分别为92.18%及93.15%.     

黔产山香草挥发油化学成分的GC-MS分析

分析黔产山香草挥发油的化学成分。采用微波萃取和水蒸气蒸馏两种方法提取山香草挥发油,运用气相色谱-质谱联用技术(GC-MS)对挥发油成分进行分离鉴定,并采用面积归一化法确定各成分的相对百分含量。水蒸气蒸馏法鉴定了39种成分,占挥发油总成分的91.44%;微波萃取法鉴定了55种成分,占挥发油总量的88.77%。实验结果为山香草的开发利用提供了理论依据。     

花椒挥发油的定性鉴别研究

采用水蒸气蒸馏法对不同产地的花椒进行挥发油提取,薄层层析法以及气相色谱-质谱联用技术进行鉴别。通过归一化法测定已鉴定成分占挥发油中的百分含量。     

罗替戈汀微球体外释放度的检查方法

分别采用摇床法和流通池法测定罗替戈汀微球的体外释放度,并通过与体内药动学曲线拟合进行选择.结果表明,摇床法和流通池法测定的体外释放度均与体内吸收具有明显相关性,相关系数r分别为0.9937和0.9978,且流通池法可检测到微球存在的较小突释.摇床法和流通池法均可用于罗替戈汀微球的体外释放度检查,流通池法作为一种新型溶出...     

声表面波气相色谱快速定性分析姜黄挥发油*

应用声表面波气相色谱快速定性分析姜黄挥发油。声表面波气相色谱采用DB-5毛细管色谱柱,初始温度45℃,6℃/s程序升温至160℃,检测结果与气相色谱质谱结果进行比较。姜黄挥发油定性分析中, 声表面波气相色谱20s完成检测,而气相色谱-质谱需要30min完成,声表面波气相色谱检测更高效;同时,声表面波气相色谱与气相色谱质谱共同检测出姜黄挥发油中10种化学成分,且10种化学成分相对百分含量总和占挥发油总成分的90%以上,由于色谱柱长度区别,声表面波气相色谱检出的化学成分相对较少;定量分析中,对声表面波气相色谱进样方式进行了考察,顶空进样与液体进样对化学成分相对百分含量检测有较大差异;采用与气相色谱质谱一致的液体进样方式,对姜黄挥发油中反式石竹烯定量分析,声表面波气相色谱最低检出限可以达到16.9 pg,在0.001624~0.01624 mg/mL范围内R=0.9976具有较好的线性关系,且精密度和重复性较好。声表面波气相色谱能够用于姜黄挥发油的快速定性和定量分析,为中药挥发油的分析提供了新的快捷的检测技术基础。     

声表面波气相色谱仪快速定性分析姜黄挥发油

应用声表面波气相色谱仪快速定性分析姜黄挥发油。声表面波气相色谱仪采用DB-5毛细管色谱柱,初始温度45℃,按6℃/s程序升温至160℃,将检测结果与气相色谱-质谱仪结果进行比较。在姜黄挥发油定性分析中,声表面波气相色谱仪20 s完成检测,而气相色谱-质谱仪需要30 min完成,声表面波气相色谱仪检测更高效;同时,声表面波气相色谱仪与气相色谱-质谱仪共同检测出姜黄挥发油中10种化学成分,且10种化学成分相对百分含量总和占挥发油总成分的90%以上,由于色谱柱长度区别,声表面波气相色谱仪检出的化学成分相对较少;定量分析中,对声表面波气相色谱仪进样方式进行了考察,顶空进样与液体进样对化学成分相对百分含量检测有较大差异;采用与气相色谱-质谱仪一致的液体进样方式,对姜黄挥发油中反式石竹烯定量分析,声表面波气相色谱仪最低检出限可以达到16.9 pg,在0.001624～0.01624 mg/mL范围内R=0.9976具有较好的线性关系,且精密度和重复性较好。声表面波气相色谱仪能够用于姜黄挥发油的快速定性和定量分析,为中药挥发油的分析提供了新的快捷的检测技术基础。     

油茶皂苷-干酪素控释片的制备及其性能研究

以油茶皂苷为主药,采用干酪素和瓜尔豆胶为控释辅料,制备油茶皂苷-干酪素控释片。研究油茶皂苷-干酪素片中油茶皂苷含量的测定方法、溶出介质对油茶皂苷-干酪素控释片释放度的影响及油茶皂苷-干酪素控释片的红外光谱,并对油茶皂苷-干酪素片体外释放动力学方程进行拟合。用香草醛-浓硫酸显色法测定pH 6.8的磷酸盐缓冲溶液作为释放介质时油茶皂苷-干酪素片中油茶皂苷的含量,回收率为98.59%。油茶皂苷-干酪素控释片在pH 6.8的磷酸盐缓冲液中,释放时间分别为3,6和12h时,其释放度分别为:23.80%,51.26%和94.77%。体外释药曲线与零级方程拟合相关性较好,相关系数(R2)为0.996。油茶皂苷、干酪素和瓜尔豆胶之间可能形成了化学键。     

蒙青绢蒿挥发油化学成分分析

采用水蒸气蒸馏法从蒙青绢蒿中提取挥发油,气相色谱-质谱法峰面积归一化法计算各成分的百分含量。从挥发油中共鉴定出50种化合物,占挥发油总量的94.11%。主要成分:3,3,6-三甲基-1,5-庚二烯-4-醇(67.83%),2,3,6-三甲基-1,4-庚二烯-6-醇(8.70%),桉树脑(2.37%),银香菊(2.12%),柠檬醇(1.91%),1-甲醇基-2,2-二甲基-3-异丁烯基-环丙烷(1.62%),乙酸-3,7-二甲基-2,6-辛二烯酯(1.14%)等。本实验首次采用GC-MS对蒙青绢蒿中挥发油化学成分进行了分析,可为该植物挥发油的开发利用提供理论依据。     

超临界CO2法萃取羌活挥发油及其成分的GC-MS分析

采用超临界CO2法萃取同一产地不同商品等级羌活中的挥发油,并用气相色谱-质谱联用技术(GC-MS)对其进行分离、鉴定,用峰面积归一法确定各组分的相对含量.结果表明,蚕羌、竹节羌、大头羌、条羌和须根中挥发油含量分别为21.8％、21,2％、19.4％、17.3％、20.8％,分别鉴定出61、65、60、60、55种成分,其中共有成分37种,且均以4-甲氧基-6-(2-丙烯基)-胡椒环、β-蒎烯、4-乙烯基-2-甲氧基-苯酚、α-蒎烯、乙酸龙脑酯、萜烯等为主要成分.不同商品等级羌活挥发油在得率、化学成分组成及含量上存在一定差异,但主要成分基本一致.除须根外,蚕羌、竹节羌、大头羌和条羌中挥发油含量依次降低,与传统等级划分方法基本一致.     

玉米胚芽胚乳中油水动态行为的NMR研究

应用核磁共振时域二维弛豫相关谱分析的方法,对玉米胚芽的核磁共振弛豫特性进行了研究.对以下三种样品进行了测定:(1)胚芽不含油(用化学方法蒸馏出)但是含有不同百分含量的水;(2)胚芽不含水(真空蒸发)但是含有不同百分含量的油;(3)含有不同百分含量的水的胚乳水系统.研究表明随着水含量的增加水的纵向弛豫时间T₁减小,表明水与胚芽基质具有强烈的相互作用,而油的纵向弛豫时间T₁随着油含量的增加变化很小,表明油与胚芽基质之间没有大的相互作用,油几乎独立地处在胚芽中;对低水分(少于5%)玉米胚芽水系统,结果表明水是束缚于胚芽基质上,而油则是以油胞的形式存在于胚芽中.在玉米胚芽水系统中有两个T₁弛豫成分,长T₁弛豫成分从基质到水的交换率为57s^-1;从水到基质的交换率为113s^-1.短T₁成分从基质到水的交换率为245s^-1;从水到基质的交换率为821s^-1.在低水合状态下,胚乳水系统仅有一个T₁弛豫成分.胚乳到水的交换率高于37s^-1.     

光学胶粘剂

本文介绍了GGJ型光学光敏胶粘剂的主要材料、配比和主要性能。并与其他一些光学胶作了对比,结果表明,该胶可广泛地应用于各种光学仪器,尤其对大批量照相机生产更为适用。该胶毒性小,操作方便,效率高,可提高工效5倍以上。     

Adhesive forces at bimetallic interfaces

Force concepts in condensed systems have been advanced significantly in the recent years. In the context of bimetallic interfaces we consider the Pauli-Hellmann-Feynman theorem, use it to check the variational calculations of interfacial energies and estimate the force constants.     

Adhesive fracture of heterogeneous interfaces

We have studied the effect of interface heterogeneity on fracture, at both local and global scales. The single cantilever beam adhesion test was used to investigate interfacial fracture between polycarbonate plates and an elastic/fragile epoxy adhesive. Two surface treatments were applied to a (given) polycarbonate plate giving zones of strong and weak adhesion parallel to the crack direction. Calculated fracture energies differed from those expected from a simple rule-of-mixtures. A perturbation method, proposed by Rice, was used and results compared with crack fronts observed in situ. The technique was applied successfully but the difference in values of stress intensity factor between the zones was found substantially different from the experimental value. In an attempt to explain discrepancies, specimens with discontinuous crack fronts (adhesive and/or plates severed along the strong/weak adhesion frontier) were tested. Good agreement was found with the rule-of-mixtures predictions raising questions about the role of crack front continuity in load transfer.     

ICP-AES法测定快干胶中硼的研究

本文探讨了ＩＣＰ－ＡＥＳ法测定快干胶中硼的方法,选择了合适的测定条件,并有效地克服了测定过程中的“记忆效应”,以石英氧瓶燃烧法分解快干胶试样,有效地避免了硼的污染和逸失。该法简便,快速。实际样品测定的相对标准偏差为１０％,回收率为９１％￣９６％。     

Metal interfaces: Adhesive energies and electronic barriers

We report a fully self-consistent calculation of the electron number density, barrier height and adhesive energy as a function of separation in an aluminium-aluminum (100) contact. The local density approximation is used for exchange and correlation. The electron number density and barrier heights are strong functions of the separation. The range of strong chemical bonding is about 0.2 nm.     

填料导热胶粘剂的性能研究

以石墨、铜粉、铝粉三种导热填料填充到环氧树脂中制备导热胶粘剂,采用SEM和金相显微镜对材料进行形貌表征,采用TPS 2500导热系数测定仪测试样品的导热系数。研究了这三种类型导热填料在不同填充量时的热导性能的变化规律,并对比讨论了三种填料在最大填充比例时胶粘剂的导热系数。     

An Investigation into the Migration of Segments in Crosslinked Fluorinated Polyimide Adhesive

Crosslinked fluorinated polyimides (CFPI) were successfully synthesized to study and explore the effect of cross-linkage on the migration of fluorinated segments and on the adhesion strength. Characterization by dynamic thermomechanical analysis (DMA) and thermo gravimetric analysis (TGA) confirmed good thermal properties of CFPI. X-ray photoelectron spectroscopy (XPS) results showed that the ratio of fluorinated component (6FDA-ODA) concentration of the surface to the bulk decreased with the crosslink density. The water contact angle of CFPI was lower than that of non-crosslinked fluorinated polyimide, indicating that the migration of fluorinated groups to the surface was reduced by the presence of cross-linkage. Therefore, CFPI, with no fluorine segregation on the surface, exhibited excellent wetting of adherent surfaces and adhesion strength, which was proved by lap shear strength (LSS) measurements and scanning electron microscopy.     

Adhesive contact: from atomistic model to continuum model

Two types of Lennard-Jones potential are widely used in modeling adhesive contacts. However, the relationships between the parameters of the two types of Lennard-Jones potential are not well defined. This paper employs a self-consistent method to derive the Lennard-Jones surface force law from the interatomic Lennard-Jones potential with emphasis on the relationships between the parameters. The effect of using correct parameters in the adhesion models is demonstrated in single sphere-flat contact via continuum models and an atomistic model. Furthermore, the adhesion hysteresis behaviour is investigated, and the S-shaped force-distance relation is revealed by the atomistic model. It shows that the adhesion hysteresis loop is generated by the jump-to-contact and jump-off-contact, which are illustrated by the S-shaped force-distance curve.