Lin Xiaojian, Gong Rujin, Li Jiaxu, Li Ping, Yu Jianguo, Rodrigues Alirio E
State Key Laboratory of Chemical Engineering, College of Chemical Engineering, East China University of Science and Technology, Shanghai, 200237, China.
State Key Laboratory of Chemical Engineering, College of Chemical Engineering, East China University of Science and Technology, Shanghai, 200237, China.
J Chromatogr A. 2016 Oct 7;1467:347-355. doi: 10.1016/j.chroma.2016.08.031. Epub 2016 Aug 12.
The separation of aminoglutethimide enantiomers by the continuous multicolumn chromatographic processes were investigated experimentally and theoretically, where the columns were packed with cellulose tris 3,5-dimethylphenyl-carbamate stationary phase (brand name Chiralcel OD) and mobile phase was a mixture of n-hexane and ethanol with monoethanolamine additive. The continuous enantioseparation processes included a synchronous shifting process (SMB) and an asynchronous shifting process (VARICOL), which allowed reducing the column number (here from six-column SMB to five-column VARICOL process). Transport-dispersive model with the consideration of both intraparticle mass transfer resistance and axial dispersion was adopted to design and optimize the operation conditions for the separation of aminoglutethimide enantiomers by SMB process and VARICOL process. According to the optimized operation conditions, experiments were carried out on VARICOL-Micro unit using five-column VARICOL process with 1/1.5/1.5/1 configuration and six-column SMB process with 1/2/2/1 configuration. Products of R-aminoglutethimide (R-AG) enantiomer and S-aminoglutethimide (S-AG) enantiomer with more than 99.0% purity were obtained continuously from extract stream and raffinate stream, respectively. Furthermore, the experiemntal data obtained from five-column VARICOL process were compared with that from six-column SMB process, the feasibility and efficiency for the separation of guaifenesin enantiomers by VARICOL processes were evaluated.
通过连续多柱色谱法分离氨鲁米特对映体的过程进行了实验和理论研究，其中色谱柱填充有三（3,5 - 二甲基苯基）氨基甲酸纤维素固定相（商品名Chiralcel OD），流动相为正己烷和乙醇的混合物并添加单乙醇胺。连续对映体分离过程包括同步切换过程（模拟移动床，SMB）和异步切换过程（变温变组成柱系统，VARICOL），这使得色谱柱数量得以减少（此处从六柱SMB减少到五柱VARICOL过程）。采用考虑颗粒内传质阻力和轴向扩散的传输 - 分散模型来设计和优化通过SMB过程和VARICOL过程分离氨鲁米特对映体的操作条件。根据优化后的操作条件，在VARICOL - Micro装置上使用具有1/1.5/1.5/1配置的五柱VARICOL过程和具有1/2/2/1配置的六柱SMB过程进行了实验。分别从萃取物流和萃余物流中连续获得了纯度超过99.0%的R - 氨鲁米特（R - AG）对映体和S - 氨鲁米特（S - AG）对映体产物。此外，将五柱VARICOL过程获得的实验数据与六柱SMB过程获得的数据进行了比较，评估了VARICOL过程分离愈创甘油醚对映体的可行性和效率。
