Stereoselective allyl amine synthesis through enantioselective addition of diethylzinc and [1,3]-chirality transfer: synthesis of lentiginosine and polyoxamic acid derivative

A new synthetic method for the preparation of allyl amines has been developed. The key steps of this method are enantioselective addition of diethylzinc and [1,3]-chirality transfer through the [3.3] sigmatropic rearrangement of allyl cyanates. Stereocontrolled syntheses of lentiginosine (1) and polyoxamic acid derivative 2 from a common intermediate 7 derived from D-tartaric acid (8), have been accomplished.     

激光靶心冲击波观测镜折反式光学系统设计

设计了一种激光靶心冲击波观测镜的光学系统.用反射式光学系统代替折射式光学系统,解决了普通玻璃在200 nm端透过率较低的问题.反射镜不引入色差,有利于系统在200~800 nm谱段消色差.为消系统轴外像差,反射系统选型为对称式.反射镜全部采用球面镜,为消反射镜以及平板玻璃窗带入的球差,引入校正镜(材料JGS1),在满足要求的条件下,控制折射镜的厚度,使系统色差满足瑞利判据的色差允差,得到了良好的成像质量.     

基于正常色散玻璃二级光谱的校正

利用正常色散玻璃校正二级光谱理论,给出了单个折射面二级光谱的计算法则,并应用此算法进行光学系统设计,给出了两个设计实例.系统仅使用正常色散玻璃组合,采用三组型设计结构,由三个大空气间隔的分离透镜组构成,很好地校正了二级光谱.     

用于航天的高分辨率大视场光学系统设计

设计了一种用于图像拍摄的高分辨率大视场光学系统,其结构形式为复杂化的反摄远基本型.主要光学参量为:f′=6.59 mm,2ω=62°,F数为2.2;在85 lp/mm处,MTF达到0.8,在230 lp/mm处MTF为0.46,基本达到衍射极限,光谱范围为0.486~0.656 μm.设计评价结果表明,该系统的光学性能能够满足成像质量要求,达到了大视场、高分辨率的目的.     

空间摄像机的热设计

根据空间摄像机的所处空间环境和结构特点,对其进行了热设计.采用被动热控措施进行热隔离和热疏导,充分利用了摄像机所搭载的卫星平台的热容;采用主动热控措施进行温差补偿,将温度拉平至热控指标范围之内.根据所采用的热控措施,针对空间摄像机进行了仿真分析,得到了满意的结果.     

部分析因设计法优化分散聚合制备单分散种子微球

采用分散聚合法,以正丁醇为分散介质、苯乙烯为单体、聚乙烯吡咯烷酮(PVP)为分散剂、偶氮二异丁腈(AIBN)为引发剂,制备单分散聚苯乙烯微球作为色谱填料的种子。实验以微球的平均粒径为主要考察指标,以GSD为次要考察指标,通过部分析因设计,获得了粒径为10μm的单分散(GSD=1.06)微球。     

点阵材料微极连续介质模型的应力优化设计

在将二维周期性点阵类材料等效为具有非局部化本构的微极连续介质的基础上,运用优化技术,探讨了基于材料相对密度和微单胞特征尺度两类变量的优化结构应力的方法,给出了针对最小化结构关键部位应力、结构最大应力最小化、最大化结构关键部位安全储备三类特定目标的结构与材料一体化协同优化结果．利用圆板小孔应力集中的数值算例验证了方法的有效性．     

低压涡轮内部流动及其气动设计研究进展

随着高空无人飞行器研究的不断升温, 高空低雷诺数条件下动力装置的研究越来越受到人们的重视.结合近年来国内外相关领域的研究工作, 对低雷诺数低压涡轮内部复杂流动机理的研究进展进行了介绍, 包括低雷诺数情况下低压涡轮内部非定常流动的特点, 叶片边界层分离及转捩现象机理, 上游周期性尾迹与下游叶片边界层相互作用机理等. 在此基础上给出了适合低雷诺数条件的低压涡轮气动设计方法:尾迹通过与边界层的相互作用, 能够抑制分离, 进而减小叶型损失, 在气动设计中有效引入非定常效应可以大幅度提高低压涡轮的气动负荷或降低气动损失, 最终达到提高性能的目的;数值及实验结果验证了这种设计方法的有效性.      

An Experimental Design Approach to Quantitative Expression for Quality Control of a Multicomponent Antidiabetic Formulation by the HILIC Method

A rapid and reproducible hydrophilic liquid chromatography (HILIC) process was established for concomitant determination of remogliflozin etabonate (RE), vildagliptin (VD), and metformin (MF) in a formulation. A face-centered central composite experimental design was employed to optimize and predict the chromatographic condition by statistically studying the surface response model and design space with desirability close to one. A HILIC column with a simple mobile phase of acetonitrile (65% v/v) and 20 mM phosphate buffer (35% v/v, pH 6, controlled with orthophosphoric acid) was used to separate RE, VD, and MF. RE, VD, and MF were separated in 3.6 min using an isocratic mode mobile phase flow at a flow rate of 1.4 mL at room temperature, and the analytes were examined by recording the absorption at 210 nm. The developed HILIC method was thoroughly validated for all parameters recommended by ICH, and linearity was observed in the ranges 20–150 µg/mL, 10–75 µg/mL, and 50–750 µg/mL for RE, VD, and MF, respectively, along with excellent regression coefficients (r² > 0.999). The calculated percentage relative deviation and relative error ascertained the precision and accuracy of the method. The selectivity and accuracy were further confirmed by the high percentage recovery of added standard drugs to the formulation using the standard addition technique. The robustness of the HILIC processes was confirmed by developing a half-normal probability plot and Pareto chart, as the slight variation of a single factor had no significant influence on the assay outcomes. Utilization of the optimized HILIC procedure for concurrent quantification of RE, VD, and MF in solid dosage forms showed accurate and reproducible results. Hence, the fast HILIC method can be regularly employed for the quality assurance of pharmaceutical preparations comprising RE, VD, and MF.     

Optimization of Ultrasound-Assisted Extraction of Yields and Total Methoxyflavone Contents from Kaempferia parviflora Rhizomes

The major bioactive components of Kaempferia parviflora (KP) rhizomes, 3,5,7,3′,4′-pentamethoxyflavone (PMF), 5,7-dimethoxyflavone (DMF), and 5,7,4′-trimethoxyflavone (TMF), were chosen as the quantitative and qualitative markers for this plant material. In order to extract bioactive components (total methoxyflavones) from KP rhizomes, ultrasound-assisted extraction (UAE) was proposed as part of this study. Plackett–Burman design (PBD) and Box–Behnken design (BBD) were utilized to optimize the effects of UAE on extraction yields and total methoxyflavone contents in KP rhizomes. First, PBD was utilized to determine the effect of five independent variables on total yields and total methoxyflavone contents. The results indicated that the concentration of the extracting solvent (ethanol), the extraction time, and the ratio of solvent to solid were significant independent terms. Subsequently, BBD with three-level factorial experiments was used to optimize the crucial variables. It was discovered that the concentration of ethanol was the most influential variable on yields and total methoxyflavone contents. Optimum conditions for extraction yield were ethanol concentration (54.24% v/v), extraction time (25.25 min), and solvent-to-solid ratio (49.63 mL/g), while optimum conditions for total methoxyflavone content were ethanol concentration (95.00% v/v), extraction time (15.99 min), and solvent-to-solid ratio (50.00 mL/g). The relationship between the experimental and theoretical values was perfect, which proved that the regression models used were correct and that PBD and BBD were used to optimize the conditions in the UAE to obtain the highest yield and total methoxyflavone content in the KP rhizomes.