Enantioseparation of paroxetine intermediate on an amylose-derived chiral stationary phase by supercritical fluid chromatography

The enantioseparation of trans-3-ethoxycarbonyl-4-(4′-fluorophenyl)-1-methyl piperidine-2,6-dione (3), which is one of the important racemic precursors of trans-(−)-paroxetine, has been investigated using supercritical fluid chromatography on a Daicel Chiralpak AD column. Supercritical CO₂ modified with methanol, ethanol and 2-propanol were used as mobile phase. The influence of type and concentration of alcohol modifier on retention factor, enantioselectivity and resolution were studied. Among methanol, ethanol and 2-propanol, 2-propanol was proved to be the most favorable modifier, and 9.5% (v/v) of 2-propanol was the preferred concentration at which racemate 3 could be separated with resolution of 15.86 and retention factor of 6.323. The effects of pressure and temperature were investigated at 9.5% (v/v) of 2-propanol in the pressure range of 12–24 MPa and temperature range of 303.15–318.15 K. It was found that the lower pressure and temperature were favorable to the enantioseparation. Using van’t Hoff plot, the isoenantioselective temperature was calculated to be 410 K. The enantioseparation process was “enthalpically driven” under experimental conditions. Finally, the retention factors were satisfactorily correlated by a simplified lattice–fluid model with average absolute relative deviation (AARD%) of both enantiomers smaller than 1.76%.     

LC Separation and Quantification of Tocopheryl Polyethylene Glycol Succinate and Tocopheryl Acid Succinate in TPGS Reaction Mixture

An analytical method was proposed for the determination of d-α-tocopheryl polyethylene glycol 1,000 succinate (TPGS 1000) and d-α-tocopheryl acid succinate (TAS) in TPGS reaction mixture with a simple and inexpensive reversed-phase liquid chromatographic method. The LC separation was carried out on a C18 analytical column with UV detection at 284 nm using acetonitrile and water (90:10, v/v) with 0.5% acetic acid (pH 3.73) at a flow rate of 1.5 mL min^?1. The average recoveries of TPGS were between 95.41 and 96.82%, while those of TAS were between 96.69 and 102.39%. Within-day and day-to-day relative standard deviations of TPGS were less than 0.23 and 0.29%, while those of TAS were less than 0.17 and 0.27%. The content of TPGS was determined in terms of the hydrolyzed α-tocopherol. The alkaline hydrolysis process demonstrated high α-tocopherol recoveries between 98.78 and 103.05%. This method has been applied successfully to the accurate determination of TAS and TPGS in highly complex reaction mixture to monitor the reaction process progress.     

合肥光源交错刀片型光位置检测器的研制

为了减小同步光尺寸对同步光位置检测器灵敏度的影响,合肥光源新研制了一种交错刀片型光位置检测器,并使用成熟的商业化产品Libera Photon进行后续的数据处理和输出。基于传统计算光位置信号的差比和方法,提出了比值和对数比两种新的计算方法,理论模拟了3种计算方法下交错刀片型光位置检测器的性能。在线标定结果与理论计算结果相符,并在机器研究光束线进行了初步的应用研究。     

一类混合Ramsey数

设a(G)表示图G的点荫度,m为正整数,H为连通图,混合Ramsey数v(a;m;H)被定义的为最小的正整数P,使得对任意P阶图G则有a(G)≥m或者H包括于G^-。本文给出了v(a;m;H)的一种计算方法,并对图Cn和轮Wn确定了v(a;n;Cn)和v(a;m;Wn)的值。     

基于四象限光位置检测器的同步光位置测量系统

为了克服现有双丝型检测器无法进行水平、垂直两个方向同时测量同步光位置的缺点,合肥光源新研制了基于四象限光位置检测器的同步光位置测量系统,并使用对数比处理技术进行后续的数据处理。通过分别对光学成像系统和四象限光位置检测器的标定,最终得到基于四象限光位置检测器的光位置测量系统的性能参数为:水平方向灵敏度0.471 2 mm-1,线性范围为±1.83 mm,垂直方向灵敏度0.635 0 mm-1,线性范围±1.32 mm。与合肥光源现有的光位置测量系统相比,具有较高的性价比。     

一种非正交对称条带束流位置监测器设计

介绍了一种条带束流位置监测器（BPM）的设计与仿真方法。在国家同步辐射实验室“太赫兹近场高通量材料物性测试系统”工程项目中,针对波荡器出口处真空室非正交对称性的问题,设计了矩形真空室和跑道形真空室下的两种非正交对称性条带BPM,并与传统的圆形真空室下条带BPM进行对比。基于边界元法,利用MATLAB软件分别对三种真空室下的条带BPM进行建模和仿真。仿真结果表明：相对于传统的圆形真空室下条带BPM,矩形和跑道形真空室下条带BPM灵敏度提高了30%,阻抗匹配误差相对降低了20%,束流位置拟合误差降低了80%。考虑加工精度,矩形真空室下的条带BPM更适用于该工程。     

合肥光源逐束团相位测量及纵向不稳定性诊断

为了研究储存环束流多束团纵向运动特性,在合肥光源（HLS-II）上研制了一套逐束团相位测量系统。该系统利用示波器直接采集BPM和信号,采用过零点检测法、时间差分（Temporal Difference, TD）法相结合的方法从BPM和信号中提取出逐束团相位。介绍了逐束团相位测量系统的系统构架、相位提取方法以及在HLS-II上的一些实验结果。通过对该系统记录的5 ms时间长度的逐束团多圈相位数据的离线分析,得到多束团纵向运动的同步振荡的频率、纵向工作点、束团振荡的模式信息以及振荡模式增长率等特征信息,诊断出HLS-II在top-off恒流运行期间存在2个较强的纵向耦合束团不稳定模式,并提取出了2个振荡模式的增长率。该系统的逐束团相位测量结果及相关纵向不稳定性分析可为机器研究、纵向反馈系统调试评估及高频RF系统的性能评估等提供参考。     

关于图的团符号控制数

引入了图的团符号控制的概念,给出了n阶图G的团符号控制数γks(G)的若干下限,确定了几类特殊图的团符号控制数,并提出了若干未解决的问题和猜想.     

Enantioseparation of racemic paroxol on an amylose‐based chiral stationary phase by supercritical fluid chromatography

The separation of racemic paroxol, a key precursor of trans‐(?)‐paroxetine, on Chiralpak AD‐H, an amylose‐based chiral stationary phase, by supercritical fluid chromatography was studied. Pulse experiments were investigated using supercritical carbon dioxide modified with methanol (MeOH), ethanol and 2‐propanol at 35°C and 15 MPa. Retention and separation factors were determined under analytical conditions for different mobile phase compositions. Among the modifiers used, MeOH was shown to be the best additive, and 5% v/v of MeOH was the preferable concentration at which selectivity of 1.14 and resolution of 3.0 was obtained. In order to evaluate the potential with respect to preparative separations, the adsorption isotherms of individual enantiomers of paroxol were estimated using the elution by characteristic point method. Isotherm parameters were determined from the overloaded elution profiles that were collected at pressure ranging from 15 to 24 MPa. The isotherms obtained were further validated by comparing experimentally recorded elution profiles with the predictions based on the equilibrium‐dispersive model. The results are important to the process design and optimization of preparative supercritical fluid chromatography application.     

Co含量对Pr10Fe74-xCo10+xC4B4 (x=0,2,4,6,8) 快淬条带的磁性能的影响

用快淬方法制备了Pr10Fe74-xCo10+xC4B4 (x=0,2,4,6,8) 条带,研究了成分和工艺对条带磁性能的影响.实验发现,当x=2,带速是20 m·s-1时,条带的磁性能最佳,其剩磁Jr=0.94 T,矫顽力μ0 iHc=0.96 T,最大磁能积 (BH)max=127.32 kJ·m-3.通过Henkel-plot分析,发现x=2,带速为20 m·s-1的样品中的晶间交换作用最强,因而能获得最佳的磁性能.