泡腾保健品中维生素E的高效液相色谱法测定

采用反相 Apollo C1 8柱 ,甲醇 /水 (98/ 2 ,V/ V)为流动相 ,流速为 0 .8m L / min,检测波长为 2 92 nm,建立了一种测定泡腾保健品 (大豆异黄酮 VE VC)中 VE的高效液相色谱测定方法。VE在浓度为 0 .0 5 38—0 .4 30 4 mg/ m L内有良好的线性关系 ,回归方程为 y=4 .87× 1 0 6x 7.1 2× 1 0 4(r=0 .9999) ,平均回收率98.0 9%。该法简便、快速、准确。     

高效液相色谱法测定富马酸异哌丙吡仑

采用高效液相色谱法测定富马酸异哌丙吡仑的含量。色谱柱为 DIKMATMRPC18(4 .6 mm× 2 0 cm,5 μm) ,流动相为乙腈 - 0 .5 %十二烷基硫酸钠 -三乙胺 (5 5∶ 4 5∶ 0 .2 ) ,用冰醋酸调 p H值至 7.0± 0 .1;流速为 1.0 m L/ min,检测波长为 2 6 5 nm。该方法回收率为 99.8% ,RSD=0 .4 4%。富马酸异哌丙吡仑在浓度为0 .0 5 92 8— 0 .1383mg/ m L范围内线性关系良好。相关系数为 r=0 .9997。该方法操作简便 ,结果准确可靠。     

液相型原子力显微镜的研制及其应用

讨论了液相型原子力显微镜(AFM)的液相探头、液体池、图像扫描处理软件以及扫描与光电反馈控制电路系统.利用该液相型AFM分别进行了气相和液相环境中的样品表面形貌测量,给出了理想的图像结果.实验表明,该液相型AFM具有优良的液相扫描性能,同时保持了很高的图像分辨率、稳定性和重复性.     

液相色谱-串联质谱同时测定动物组织中22种同化激素

采用高效液相色谱-电喷雾串联质谱仪(LC-ESI-MS-MS),在多反应监测(MRM)模式下建立了动物组织中甾体类和1,2-二苯乙烯类22种同化激素(睾酮、甲基睾酮、丙酸睾酮、苯丙酸诺龙、勃地龙、康力龙、群勃龙、醋酸群勃龙、丙酸诺龙、大力补、醋酸甲羟孕酮、诺龙、孕酮、甲炔诺酮、甲羟孕酮、雌酮、雌二醇、雌三醇、炔雌醇、己烷雌酚、己烯雌酚、双烯雌酚)的快速确认测定方法.试样中的药物经叔丁基甲醚提取后,过C18固相萃取柱净化,氮吹至干,用1 mL乙腈/水(1:1,V/V)定容后测定.采用正离子扫描和负离子扫描的方式进行仪器方法学研究,确定丰度比最高的2对离子作为监测离子,进行MRM模式定性定量分析.该方法的检出限(LOD)为0.2～0.5 μg/kg,定量限(LOQ)为0.5～1.0 μg/kg;在2.0～200.0 μg/L的线性范围,相关系数r均大于0.998.在1.0 μg/kg的添加水平上,上述22种激素的平均回收率为56.2%～112.3%,相对标准偏差为2.6%～13.2%.本法操作简单,灵敏度高,可用于动物组织中22种同化激素的残留测定.     

A simple and generalized model for predicting the density of ionic liquids

A simple and accurate model to predict the density of ionic liquids is presented. The proposed model is based on a generalized correlation that has been conveniently modified and experimental literature data have been used to fit the five model parameters, to finally propose an equation that allows predicting densities of any ionic liquid. The model uses the critical temperature, the critical volume, the normal boiling temperature and the molecular mass to estimate the density at temperatures commonly used in ionic liquid applications (270–360 K). A set of 602 density data for 146 ionic liquids has been used in the study. The results were compared with predictions of ten generalized corresponding states principle correlations available in the literature. These generalized correlations have not been applied to ionic liquids before so the appropriateness and accuracy of these models to ionic liquid density estimation are unknown until now. Results show that the new simple correlation gives low deviations and can be used with confidence in thermodynamic and engineering calculations.     

Controlled self-assembly of chiral gelator molecules into aligned fibers induced by nematic to smectic B phase transitions

Chiral bisoxalamide 1 shows remarkable gelling capacity of the nematic and smectic B liquid-crystalline phases of heptylcyclohexanecarboxylic acid (HCCA). Chiral nematic-containing left-handed helical fiber bundles are formed if the gelator is present in amounts higher than 0.55 wt %. With lower amounts of 1, no nematic gel forms, however, a nematic to smectic B phase transition triggers instantaneous self-assembly of gelator molecules into aligned fibers. The latter liquid crystalline gel system represents an example of controlled self-assembly induced by a liquid crystalline phase transition.     

Synthesis and characterization of cross-conjugated cruciforms with varied functional groups

A series of novel oligo(p-phenylenes) (OPPs) derivatives with bisdiene side-chains are synthesized and fully characterized. These cruciforms are soluble in common organic solvents and show good thermal stability. Absorption and emission spectra are recorded to study the effect of different electron-withdrawing and electron-donating groups on photophysical properties. Powder XRD shows crystalline structures for all the cruciforms. Single crystal XRD studies show tight-packing along the planar bisdiene axis but significant twisting along phenylene units, which correlate the role of functionalization along the bisdiene axis in tuning the band gaps of the cruciforms.     

Synthesis and properties of novel liquid crystalline materials with super high birefringence: styrene monomers bearing diacetylenes, naphthyl, and nitrogen-containing groups

Three new liquid crystal asymmetrical styrene monomers bearing diacetylenes, naphthyl, and nitrogen-containing groups were successfully synthesized from 2-(bromoethynyl)-6-(hexyloxy)naphthalene, 4-(4-bromo-2-vinylphenyl)-2-methylbut-3-yn-2-ol, and derivatives of 4-ethynylaniline. The molecular structures of these compounds were confirmed by FTIR, ¹H NMR spectroscopy, elemental analysis, and mass spectrometry. The liquid crystalline properties of monomers were characterized by differential scanning calorimetry and polarized light microscopy. Results indicated that all the compounds exhibited the nematic phase in liquid crystal state and super high optical birefringence of 0.5-0.8. The change of terminal nitrogen-containing group affected the birefringence values in the order of -N(CH₃)₂<-NH₂<-NCS. Moreover, measurements using UV-vis and fluorescence spectroscopy showed their good photoluminescence properties and high quantum efficiency of 0.4-1.0.     

Volumetric and viscosity studies of interactions between sodium phosphate salts and poly(propylene glycol) 400 in aqueous solutions at different temperatures

Density and sound velocity at the 288.15–313.15 K and viscosity at the 298.15–313.15 K temperature range at 5 K intervals for polypropylene glycol (PPG) in aqueous solutions of sodium di-hydrogen phosphate, di-sodium hydrogen phosphate and tri-sodium phosphate with salt mass fractions 0.00, 0.010 and 0.020 are reported at atmospheric pressure. From the experimental density and sound velocity data, the apparent specific volume, excess specific volume, isentropic compressibility and isentropic compressibility deviation values have been determined. The infinite dilution apparent specific volume and isentropic compressibility values of PPG have been obtained and from which the infinite dilution apparent specific volumes of transfer of PPG from water to aqueous sodium phosphate solutions have been obtained for the investigated salt concentrations and temperatures. The excess specific volume, isentropic compressibility and viscosity deviation are negative and decrease in magnitude as temperature, concentration of sodium phosphate and charge on the anion of electrolyte increases.     

Electron–ion recombination in radiation tracks in liquid argon: a computer simulation study

A simulation method is proposed to model electron–ion recombination in radiation tracks in liquid argon at 87 K. The method is applied to calculate the electron escape probability in clusters of up to 20 pairs of electrons and cations that represent a fragment of the track. The results reproduce the basic features of the track recombination in liquid argon observed in experiment.