Development of a general separation strategy by countercurrent chromatography using sanshools from Zanthoxylum bungeanum oleoresin as a case study

Three kinds of sanshools were separated from Zanthoxylum bungeanum oleoresin by high-speed countercurrent chromatography. Sanshools are a series of amide compounds extracted from the Zanthoxylum bungeanum. Due to similar structures, polarities, and dissociation constants, it was challenging to select an appropriate solvent system for their complete separation by countercurrent chromatography. To address this challenge, a solvent-system-selection strategy was proposed to identify a relatively suitable solvent system. Additionally, a separation procedure incorporating multi-elution modes selection was established to separate similar compounds in a logical order. Ultimately, a solvent system comprising n-hexane:ethyl acetate:methanol:water in a ratio of 19:1:1:5.67 was selected. Three amide compounds with high purity were obtained through the use of recycling elution mode to improve separation resolution: hydroxy-ε-sanshool (8.4 mg; purity: 90.64%), hydroxy-α-sanshool (326.4 mg; purity: 98.96%), and hydroxy-β-sanshool (71.8 mg; purity: 98.26%) were obtained from 600 mg sanshool crude extract. The summarized solvent-system-selection strategy and separation procedure incorporating multi-elution modes may instruct countercurrent chromatography users, particularly novices, seeking to separate compounds with highly similar chemical properties.     

Biphasic alcoholysis coupled with high-speed countercurrent chromatography for high performance on separating phorbol from Croton tiglium Linn extracts

Phorbol is a tetracyclic diterpenoid found in Euphorbia tirucalli, Croton tiglium, and Rehmannia glutinosa, and is nuclear of various phorbol esters. The rapid obtaining of phorbol with high purity highly contributes to its application, such as synthesizing phorbol esters with designable side chains and particular therapeutic efficacy. This study introduced a biphasic alcoholysis method for obtaining phorbol from croton oil by using polarity imparity organic solvents in both phases and established a high-speed countercurrent chromatography method for simultaneous separation and purification of phorbol. The optimized operation conditions of biphasic alcoholysis were a reaction time of 91 min, a temperature of 14°C, and a croton oil-methanol ratio of 1:30 (g:ml). The phorbol during the biphasic alcoholysis was 3.2-fold higher in content than that obtained in conventional monophasic alcoholysis. The optimized high-speed countercurrent chromatography method was using the ethyl acetate/n-butyl alcohol/water at 4.7:0.3:5 (v:v:v) with Na₂SO₄ at 0.36 g/10 ml as the solvent system, using the mobile phase flow rate of 2 ml/min, the revolution of 800 r/min, under which the retention of the stationary phase was achieved at 72.83%. The crystallized phorbol following high-speed countercurrent chromatography was obtained as high purity of 94%.     

高速运动裂纹扩展和分叉现象的近场动力学数值模拟

首先介绍了近场动力学的基本理论,然后以两个实例分析了高速运动裂纹的扩展及分叉现象.分析了近场动力学参数(邻域半径、相邻节点距)及外部参数(材料的弹性模量、密度、温度改变量)等对裂纹分叉的速度和角度的影响并进行了对比分析,数值结果表明:随着邻域半径的增大,裂纹传播速度逐渐减少而裂纹分叉角度逐渐增加;随着相邻节点间距的增加,裂纹的传播速度逐渐减少而裂纹分叉角度也逐渐减少;裂纹分叉长度偏向于弹性模量小和密度大的材料;裂纹传播速度随着弹性模量差值的增大而增大,随着密度差值的减小而增大,同时随着外界温度改变量的增大而减少.近场动力学能自发地模拟裂纹扩展和分叉,不需要借助任何外部准则,不需要预先设置裂纹扩展路径,因此它具有天然的优势.     

以能耗最低为目标的列车调控方案研究

研究的是以能耗最低为目标的单、多列车优化调控方案问题.首先根据列车运行的各个阶段的分析,构建以运行能耗最低为目标的非线性规划模型,采用逐步迭代算法进行求解,得到的最佳运行模式为无惰行运行,相应的最小能耗为12.47kwh.对于无高峰期的多列车节能运行控制问题,建立了以回收能量最多为目标的0-1非线性规划模型,得到发车间隔为578.86s、575.59s和760.89s,并以此规律循环33轮的发车间隔时间表,使得能量回收最大为250.57kwh,回收率为19.66%.对于存在早晚高峰的情形,建立了以回收能量最多为目标的5阶段0.1非线性规划模型,求出了全天的最优发车方案.     

声学脉冲序列及全透声机理研究

本文研究一维周期性层状结构中材料弹性模量时变因素作用下的声透射临界现象, 探究了这种声学脉冲序列及全透声现象的内在机理. 考虑弹性模量时变因素的影响, 通过求解波动方程, 运用分离变量法解得特征指数, 进而得到临界现象. 当调制幅值低于或等于临界值时, 周期性结构能够将入射波转化为一系列周期的毫秒级的反射脉冲序列; 尤其在调制幅值等于临界值时, 当周期性结构的层数达到16层时, 反射脉冲序列有完整的0和1 的波形; 当大于临界值时, 反射系数在50 ms内迅速衰减至0, 此时的结构相当于完全透声, 入射波可以无损地完全透过, 产生调制透声现象. 这些特殊的现象可为声波的动态控制、声脉冲序列的产生和声波的定向传播提供重要的理论依据, 在超声换能器及调制透声方面具有实际的工程应用前景.     

红外图像高速实时存储系统设计

针对红外图像具有分辨率低、帧频高的特点,以及目标特性分析和图像处理算法验证需要完整、无损记录图像数据的要求,提出了一种高速数字图像传输记录系统方案。方案采用HOTLinkⅡ＋FPGA＋PCI的体系结构,数据通过同轴线从红外图像设备传输到图像记录设备的CYP15G0101芯片,实现了远距离的点到点可靠传输和解码。FPGA和PCI接口芯片对图像数据进行接收和缓冲,工控机软件通过调用PCI SDK提供的API函数实现对PCI接口芯片的初始化、控制和数据传输等操作,从而将图像数据按照预定的格式连续地写入物理上连续的硬盘存储空间,最终实现数据记录、回放和分析等功能。该方案已经成功应用于某型红外图像记录设备并经过长时间测试,记录时间、漏记率等指标和回放等功能均满足研制要求。     

A Simple and Efficient Two-Dimensional High-Speed Counter-Current Chromatography Linear Gradient and Isocratic Elution Modes for the Preparative Separation of Coumarins from Roots of Toddalia asiatica (Linn.) Lam.

Toddalia asiatica (L.) Lam. (Rutaceae) has shown a broad spectrum of biological properties, such as anti-inflammatory, antioxidant, antimicrobial, anti-HIV, and anticancer properties. The present study is concerned with the separation of the main components with broad partition coefficients (K_D values) from T. asiatica, using linear gradient high-speed counter-current chromatography (LGCCC) combined with an off-line two-dimensional (2D) mode. Similar to the binary gradient HPLC, the LGCCC mode is operated by the adjustment of the proportion between the mobile phase of 5:5:1:9 (v/v) (pump A) and 5:5:4.5:5.5 (v/v) (pump B) in an n-hexane/ethyl acetate/methanol/water solvent system. The off-line 2D-CCC mode was used in this study for the secondary separation of two similar K_D value compounds with n-hexane/ethyl acetate/methanol/water (5:5:4:6, v/v). Notably, six coumarins, namely, tomentin (1), toddalolactone (2), 5,7,8-trimethoxycoumarin (3), mexoticin (4), isopimpinellin (5), and toddanone (6), were efficiently separated. The structures of the pure compounds were elucidated by spectral techniques and compared with the literature.     

高速离心泵轴向力平衡方法研究

根据高速离心泵轴向力产生的原因提出了平衡孔与平衡管、斜齿轮传动和平衡鼓与平衡盘的组合结构等轴向力平衡方法,通过理论分析和设计实践,得出采用平衡孔和平衡管及斜齿轮传动是简单但又实用的高速离心泵的主要轴向力平衡方法。     

波纹板结构动力学建模及其自由振动特性分析

波纹板结构是高速列车中较为常见的型材结构,因其具有轻质、高强度和高稳定性等一系列优点,所以广泛应用于车体结构轻量化设计。首先,基于一阶剪切变形理论和中厚壳(圆弧壳)理论,采用微分求积有限元法(DQFEM)建立一般边界条件下五自由度波纹板结构的通用动力学分析模型;紧接着对五自由度波纹板结构动力学模型进行收敛性验证,确定最佳微分节点数和惩罚因子的取值;然后,采用有限软件(ABAQUS)验证了建立模型的准确性;最后根据已建立模型,研究波纹板结构参数对其振动特性的影响。结果表明,波纹板结构厚度和固支边界条件会增加其固有频率,提高波纹板结构的稳定性,使得共振频率向高频移动;增加波纹板结构长度、参与耦合圆弧壳半径和参与耦合圆弧壳弧度会降低其固有频率,使得共振频率向低频移动。     

微波消解ICP-AES法测定高速工具钢中锰、磷、镍、铜、铬、钒

高速工具钢为高碳高合金工具钢,常温下样品酸溶分解较为困难。本文利用微波消解提高溶样的温度和压力,在王水、氢氟酸和硫酸介质中使样品充分消解,再用饱和硼酸溶液络合过量的氢氟酸,基体匹配消除铁基体的影响,ICP-AES法同时测定锰、磷、镍、铜、铬、钒的含量。测定高速工具钢标样,测定值与标样值相吻合,本方法的精密度在0.55%～4.06%。加标回收率在95.6%～114.8%,满足测定要求。