| Development and validation of HPLC methods for enantioseparation of mirtazapine enantiomers at analytical and semipreparative scale using polysaccharide chiral stationary phases | |
| Department | 甘肃省天然药物重点实验室 |
Zhai ZD(翟宗德); Shi YP(师彦平) ; Wang T(王婷)
| |
| 2005 | |
| Source Publication | Analytica Chimica Acta
 |
| ISSN | 0003-2670 |
| Volume | 550Pages:123–129 |
| Abstract | 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. |
| Keyword | Enantioseparation Polysaccharide Carbamate Phase Semipreparative Hplc Optical Rotation Circular Dichroism Mirtazapine |
| Subject Area | 分析化学 ; 药物化学 |
| Funding Organization | the “Bairen Jihua” Foundation of Chinese Academy of Sciences (CAS) in 2000;National Natural Science Foundation of China (NSFC No.20475057) |
| Indexed By | SCI |
| Language | 英语 |
| Funding Project | 抗糖尿病中药古方活性组份的发现及其高效液相色谱-质谱联用仪系统性研究 |
| Citation statistics | |
| Document Type | 期刊论文 |
| Identifier | http://ir.licp.cn/handle/362003/2500 |
| Collection | 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 |
| Corresponding Author | Shi YP(师彦平) |
| Recommended Citation GB/T 7714 | Zhai ZD,Shi YP,Wang T. 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 | 翟宗德,师彦平,&王婷.(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 | 翟宗德,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. |
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