Development and validation of HPLC methods for enantioseparation of mirtazapine enantiomers at analytical and semipreparative scale using polysaccharide chiral stationary phases
会议名称：《30th International Symposium on Capillary Chromatography、4th GC×GC Symposium、16th National Symposium and Exhibition on Chromatography,i.e. 1st Dalian International Symposium and Exhibition on Chromatography》
会议日期：2007年
学科分类：081704[工学-应用化学] 07[理学] 08[工学] 0817[工学-化学工程与技术] 070302[理学-分析化学] 0703[理学-化学]
关 键 词：Enantioseparation polysaccharide carbamate phase semipreparative HPLC optical rotation circular dichroism mirtazapine
摘 要：正Mirtazapine is a recent noradrenergic and specific serotonergic antidepressant（NaSSA）drug,and used to treat moderately and severely depressed hospitalized and *** HPLC methods were developed for the analytical and semipreparative resolution of new antidepressant drug mirtazapine *** analytical scale,the separation of the mirtazapine enantiomers was investigated using both cellulose and amylose tris（3,5- dimethylphenylcarbamate）（CDMPC and ADMPC）chiral stationary phases under normal-phases and polar organic *** good baseline enantioseparation was achieved in all ***,the elution order of mirtazapine enantiomic pairs was found reversed by changing the stationary phase from the amylose-based ADMPC-CSPs to its cellulose-based counterpart,*** validation of the analytical methods including linearity,limit of detection,limit of guantitation,recovery and precision,together with the semipreparative resolution of mirtazapine racemate were carried out using cellulose tris （3,5-dimethyiphenylcarbamate）chiral stationary phases and methanol as mobile phase without any basic additives under polar organic *** analytical scale,the elution times of both enantiomers were less than 6 min at room temperature and 1.0 ml/min,with the separation factor（α）1.99 and the resolution facotor（Rs）3.56. Then,the analytical methods were scaled up to semipreparative loading to obtain small amount of both mirtazapine *** semipreparative scale,about 16 mg/h enantiomers could be isolated and elution times of both enantiomers were less than 10 min at 2.0 ml/*** increase the throughput,the technique of boxcar injections was *** enantiomer（（-）-（R）-mirtazapine）was isolated with purity of 99.9% *** 98.0% yield and another（（+）-（S）-mirtazapine）was isolated with purity of 97.0% *** 99.0% *** addition,optical rotation and circular dichroism spectroscopy of both mirtazapine enantiomers isolated were also investi