One unknown impurity （Imp-II） during the analysis of laboratory batches of isoproterenol hydrochloride was detected in the level ranging from 0.04% to 0.12% by high performance liquid chromatography with UV detectio...One unknown impurity （Imp-II） during the analysis of laboratory batches of isoproterenol hydrochloride was detected in the level ranging from 0.04% to 0.12% by high performance liquid chromatography with UV detection. The unknown impurity structure was proposed as 4-[2-（propan-2oylamino）ethyl]benzene-l,2-diol （Imp-II） using the liquid chromatography-mass spectrophotometry （LC-MS） analysis. Imp-II was isolated by semi-preparative liquid chromatography from the impurity-enriched reaction crude sample. Its proposed structure was confirmed by nuclear magnetic spectroscopy such as 1H, 13C, DEPT （1D NMR）, HSQC （2D NMR） and infrared spectroscopy （IR）, and retention time and purity with HPLC followed by the chemical synthesis. Due to less removable nature of Imp-II during the purification, the synthetic process was optimized proficiently to control the formation of Imp-II below to the limit 〈 0.12% in the course of reaction. The new chemical route was developed for the preparation of this impurity in required quantity with purity to use as reference standard. The most probable mechanism for the formation of Imp-II was discussed in details.展开更多
合成了均苯四甲酸酐修饰β-环糊精微球,通过红外光谱、X-射线光电子能谱、扫描电镜对其进行结构和形貌表征,获得了大小均匀、表面光滑、粒径为5~10μm的微球。以该微球为手性固定相,采用溶胶-凝胶法制备了颗粒固定化整体柱,并考察了柱...合成了均苯四甲酸酐修饰β-环糊精微球,通过红外光谱、X-射线光电子能谱、扫描电镜对其进行结构和形貌表征,获得了大小均匀、表面光滑、粒径为5~10μm的微球。以该微球为手性固定相,采用溶胶-凝胶法制备了颗粒固定化整体柱,并考察了柱制备过程中的影响因素,获得最佳的柱制备条件：聚乙二醇∶冰乙酸∶正硅酸甲酯为0.25 g∶2.5 m L∶1.5 m L,溶胶∶微球为2 m L∶1 g,水浴时间10 h,水浴温度40℃。利用该颗粒固定化整体柱对盐酸异丙肾上腺素和盐酸氯丙那林对映体进行手性拆分,达到了基线分离。展开更多
文摘One unknown impurity （Imp-II） during the analysis of laboratory batches of isoproterenol hydrochloride was detected in the level ranging from 0.04% to 0.12% by high performance liquid chromatography with UV detection. The unknown impurity structure was proposed as 4-[2-（propan-2oylamino）ethyl]benzene-l,2-diol （Imp-II） using the liquid chromatography-mass spectrophotometry （LC-MS） analysis. Imp-II was isolated by semi-preparative liquid chromatography from the impurity-enriched reaction crude sample. Its proposed structure was confirmed by nuclear magnetic spectroscopy such as 1H, 13C, DEPT （1D NMR）, HSQC （2D NMR） and infrared spectroscopy （IR）, and retention time and purity with HPLC followed by the chemical synthesis. Due to less removable nature of Imp-II during the purification, the synthetic process was optimized proficiently to control the formation of Imp-II below to the limit 〈 0.12% in the course of reaction. The new chemical route was developed for the preparation of this impurity in required quantity with purity to use as reference standard. The most probable mechanism for the formation of Imp-II was discussed in details.
文摘合成了均苯四甲酸酐修饰β-环糊精微球,通过红外光谱、X-射线光电子能谱、扫描电镜对其进行结构和形貌表征,获得了大小均匀、表面光滑、粒径为5~10μm的微球。以该微球为手性固定相,采用溶胶-凝胶法制备了颗粒固定化整体柱,并考察了柱制备过程中的影响因素,获得最佳的柱制备条件：聚乙二醇∶冰乙酸∶正硅酸甲酯为0.25 g∶2.5 m L∶1.5 m L,溶胶∶微球为2 m L∶1 g,水浴时间10 h,水浴温度40℃。利用该颗粒固定化整体柱对盐酸异丙肾上腺素和盐酸氯丙那林对映体进行手性拆分,达到了基线分离。
