Development and validation of HPLC methods for enantioseparation of mirtazapine enantiomers at analytical and semipreparative scale using polysaccharide chiral stationary phases
文献类型：期刊论文
| 作者 | Shi YP(师彦平) ; Shi YP(师彦平)
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| 刊名 | Analytica Chimica Acta
 |
| 出版日期 | 2005 |
| 卷号 | 550页码:123–129 |
| 关键词 | Enantioseparation Polysaccharide carbamate phase Semipreparative HPLC Optical rotation Circular dichroism Mirtazapine |
| ISSN号 | 0003-2670 |
| 通讯作者 | 师彦平 |
| 中文摘要 | Novel HPLC methods were developed for the analytical and semipreparative resolution of new antidepressant drug mirtazapine enantiomers. At 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 modes. Good baseline enantioseparation was achieved using cellulose tris(3,5-dimethylphenylcarbamate) chiral stationary phases under both normal-phases and polar organic modes. Furthermore, 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, CDMPC–CSPs. The validation of the analytical methods including linearity, limit of detection (LOD), limit of quantification (LOQ), recovery and precision, together with the semipreparative resolution of mirtazapine racemate were carried out using cellulose tris(3,5-dimethylphenylcarbamate) chiral stationary phases and methanol as mobile phase without any basic additives under polar organic mode. At analytical scale, the elution times of both enantiomers were less than 6 min at normal temperature and 1.0 ml/min, with the separation factor (α) 1.99 and the resolution factor (Rs) 3.56. Then, the analytical methods were scaled up to semipreparative loading to obtain small quantities of both mirtazapine enantiomers. At 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/min. To increase the throughput, the technique of boxcar injections was used. One enantiomer ((−)-(R)-mirtazapine) was isolated with purity of >99.9% e.e. and >98.0% yield and another ((+)-(S)-mirtazapine) was isolated with purity of >97.0% e.e. and >99.0% yield. In addition, optical rotation and circular dichroism (CD) spectroscopy of both mirtazapine enantiomers isolated were also investigated. |
| 学科主题 | 分析化学 ; 药物化学 |
| 收录类别 | SCI |
| 资助信息 | the “Bairen Jihua” Foundation of Chinese Academy of Sciences (CAS) in 2000;National Natural Science Foundation of China (NSFC No.20475057) |
| 语种 | 英语 |
| WOS记录号 | WOS:000232356200016 |
| 公开日期 | 2013-03-01 |
| 源URL | [http://210.77.64.217/handle/362003/2500]  |
| 专题 | 兰州化学物理研究所_中科院西北特色植物资源化学重点实验室/甘肃省天然药物重点实验室 |
| 通讯作者 | Shi YP(师彦平); Shi YP(师彦平) |
| 推荐引用方式 GB/T 7714 | Shi YP,Shi YP. Development and validation of HPLC methods for enantioseparation of mirtazapine enantiomers at analytical and semipreparative scale using polysaccharide chiral stationary phases[J]. Analytica Chimica Acta,2005,550:123–129. |
| APA | 师彦平,&师彦平.(2005).Development and validation of HPLC methods for enantioseparation of mirtazapine enantiomers at analytical and semipreparative scale using polysaccharide chiral stationary phases.Analytica Chimica Acta,550,123–129. |
| MLA | 师彦平,et al."Development and validation of HPLC methods for enantioseparation of mirtazapine enantiomers at analytical and semipreparative scale using polysaccharide chiral stationary phases".Analytica Chimica Acta 550(2005):123–129. |
入库方式： OAI收割
来源：兰州化学物理研究所
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