在高氯酸铕-二苯亚砜-邻菲罗啉三元配合物中Pr3+对Eu3+发光的影响

合成了一系列异核配合物[(Eu1-xPrx)(DPSO)(phen)3(ClO4)2]ClO4*nH2O(x=0.000～0.200, DPSO为二苯亚砜, phen为邻菲罗啉, n=1, 2, 3, 4, 5, 6). 对配合物进行了组成分析, 摩尔电导, IR光谱及荧光激发和发射光谱的测定. 荧光光谱测定结果表明 本身不发光的Pr3+对Eu3+的发光产生较大影响, 当Pr3+的掺入量为0.001 mol时, 可使Eu3+的发光强度提高到200%以上,随着Pr3+浓度的增大,对Eu3+的发光先敏化后猝灭.Eu3+在配合物中所处的格位对称性低,无对称中心.     

组合生成算法与多元线性回归相结合用于近红外光谱波长的优选

分立波长型近红外光谱分析仪是光谱分析仪器中较为普及的一种快速成份定量分析仪。如滤光片型、发光二极管型等。该类分析仪器研发的一个主要问题是如何针对于待测物质主要成份进行近红外光谱解析。找到最优定标波长组合用于建立稳健的定标模型。常用的波长选择方法为相关光谱结合逐步多元线性回归方法,该方法依据各参与定标波长所对应的t检验值进行最优定标波长的判别,但在实际应用中定标模型的定标精度和预测精度相差较大,具有很大的不准确性。为了实现定标波长的优选引入了组合数学中的组合生成算法。可以在较短的时间内完成最优波长组合的选取,结果是令人满意的。     

固定化脂质体色谱研究中药复方的细胞膜通透性成分及其质量控制

提出了固定化脂质体色谱(immobilized liposome chromatography,ILC)研究中药复方的细胞膜通透性成分及其质量控制的方法。以当归补血汤及其组分为例,考察了它们在ILC色谱柱上的分离效果;当归补血汤水提取液和75％乙醇提取液在ILC色谱柱上各有8个保留峰,当归水提取液、甲醇提取液和75％乙醇提取液在ILC色谱柱上分别有3、6、9个保留峰,黄芪水提取液、甲醇提取液和75％乙醇提取液在ILC色谱柱上各有7个保留峰;建立了当归补血汤及其组分中阿魏酸和蒿本内酯的定量分析方法,当归补血汤水提取液和75％乙醇提取液中阿魏酸的含量分别为0．0743％和0．0688％,蒿本内酯的含量分别为0．0472％和0．457％,当归水提取液和75％乙醇提取液中阿魏酸的含量分别为0．0694％和0．0691％,蒿本内酯的含量分别为0．0781％和0．455％。     

用数理统计确定回归方程的形式

从数理统计角度分析热敏电阻随温度变化的回归方程,得出的回归方程与理论公式形式一致,建议用Excel的数据分析工具对实验数据进行数理统计。     

大口径平面光学元件超精密加工技术的研究

为了解决激光核聚变装置中大口径平面光学元件的批量制造难题,将先进制造技术和传统抛光技术相结合,提出了一种新的工艺方法,即使用ELID(在线电解)磨削代替传统的铣磨和初抛工序,以提高生产效率。利用数控抛光将工件抛光至最终的面形精度,以提高生产效率和减少边缘效应。将连续抛光作为最终加工工序,使加工工件的表面粗糙度和波纹度达到工程要求。实验证明这一新的工艺方法是可行的。     

Effect of chemically bonded stationary phases and mobile phase composition on beta-blockers retention in RP-HPLC

The effects of stationary and mobile phase on retention of 18 beta-adrenolytic drugs (beta-blockers) have been studied. Four 'deactivated surface' stationary phases (polar-embedded or end-capped) were examined. Special attention was drawn to the cholesterolic (SG-CHOL) and alkylamide (SG-AP) stationary phases, and their application for analysis of the compounds. The retention of analyzed substances was also examined in terms of mobile phase composition. Sixteen different configurations of mobile phases were prepared, all based on methanol and acetonitrile with ammonium acetate and ammonium formate. The difference in retention between ammonium formate and acetate water solutions, and peak shape changes related to the addition of triethylamine (TEA), were investigated. Principal component analysis was used to find the similarities between stationary phases. Polar-embedded phases synthesized on the same sorbent possess very similar properties. All phases based on silica gel compared with the monolithic column also showed similarities in retention of beta-blockers. The addition of TEA to the mobile phase did not influence strongly the retention, and analysis of asymmetry factors showed only a little peak broadening for a few compounds on the monolithic column.     

Application of near infrared spectroscopy and multivariate data analysis for the evaluation of glue lines of untreated and copper azole treated laminated timber before and after ageing

The necessity for inspection and assessment of glued laminated timber structures in service has raised interest in the evaluation of the glue lines. Glue line spectra were analysed and are discussed in detail with respect to spectral contributions from the adhesive, the hardener, the wood lamella below the adhesive, the curing temperature as well as ageing-related spectral changes. The combination of near infrared (NIR) spectroscopy and principal component analysis (PCA) allowed distinguishing between aged and non-aged samples and different copper azole preservative treatment levels of phenol-resorcinol-formaldehyde (PRF) glue lines. NIR-based partial least squares (PLS) regression modelling was performed for the glue line shear strength and for the curing temperature. These findings show that NIR spectroscopy is a fast and useful technique to evaluate the degradation on the PRF glue lines of untreated and copper azole treated laminated timber.     

THM PyGC–MS of wood fragment and vegetable fibre forensic samples

Wood fragments and vegetable fibres were investigated using thermally assisted hydrolysis and methylation with pyrolysis gas chromatography–mass spectrometry (THM PyGC–MS). Multiple ion chromatography was used to decrease the interference from cellulosic peaks, and to obtain greater resolution between the lignin peaks. Forty-four wood samples were analysed using THM PyGC–MS. The wood fragments were able to be differentiated into angiosperms (hardwoods) and gymnosperms (softwoods) using principle component analysis (PCA), hierarchical cluster analysis (HCA), and the ratio of syringyl to guaiacyl lignin fragments (S/G ratio). PCA and HCA also differentiated several Monterey pine samples from the rest of the gymnosperms, primarily by the presence of β-pinene, an extractive compound. Other gymnosperm species and the individual angiosperm species were unable to be differentiated. A pilot study investigating the use of THM PyGC–MS for the analysis of vegetable fibres in forensic science found that the fibre types tended to group into two clusters, with one containing cotton, hemp and linen; and the other consisting of hessian, sisal, jute and coir. The seagrass sample was able to be differentiated from both groups. These groups were well separated using PCA, HCA and by the ratio of cinnamyl phenolic derivatives to guaiacyl lignin derivatives (C/G ratio). Some grouping of each fibre type was evident within each cluster, however the separation between the clusters was insufficient to differentiate them using these statistical techniques. THM PyGC–MS of vegetable fibres showed some potential for future use in forensic science.     

钙调蛋白抑制剂预测模型研究

选用30个结构多样的caM抑制剂分子作为数据集,采用多元线性回归(MLR)方法及主成分回归分析(PCA)方法对每个化合物的194个分子参数进行回归分析,分别建立了各自的最优预测模型.结果表明:多元线性回归分析方法所建模型与主成分回归所建模型相对比,发现逐步筛选法为最优建模方法?该方法所建模型统计结果良好(R2=0.952,SEE为0.289),应用于检验集时结果也比较令人满意(R2=0.941,SEP为0.295),模型表现出较强的可靠性和预测性.     

One-pot Synthesis of 1,8-Dioxo-decahydroacridine Derivatives in Aqueous Media

A new and efficient method for the synthesis of 1,8‐dioxo‐9‐aryl‐decahydroacridine derivatives was developed via a one‐pot three component reaction of dimedone, aromatic aldehydes and ammonium acetate in the presence of ammonium chloride, or Zn(OAc)₂·2H₂O or L‐proline separately in water in the short period of time and high yields.