DEVELOPMENT OF AN EFFICIENT HPLC METHOD WITH PRE-COLUMN DERIVATIZATION FOR DETERMINATION OF ENANTIOMERIC PURITY OF 2-(AMINOMETHYL)-1-ETHYLPYRROLIDINE

Journal of The Chilean Chemical Society

WANG, DAO-CAI¹  PU, LING-XIANG¹  SONG, HANG¹  QIAN, GUO-FEI¹  YAO, SHUN¹  YAO, TIAN¹ 

[1] Sichuan University, Chengdu, China

关键词: HPLC;    enantiomeric separation;    2-;    (aminomethyl)-;    1-;    ethylpyrrolidine;    pre-;    column derivatization;   

DOI  :  10.4067/S0717-97072015000100002

学科分类：化学（综合）

来源: Sociedad Chilena de Quimica

【 摘 要 】

The development of a simple and efficient analytical method for determination of enantiomeric purity of 2-(aminomethyl)-1-ethylpyrrolidine was presented. The method was based on pre-column derivatization of 2-(aminomethyl)-1-ethylpyrrolidine with 4-nitrobenzoic acid completing separation of the enantiomers on high performance liquid chromatographic (HPLC) chiral stationary phase (CSP). After optimizing all the effective parameters, the best performances were achieved on a Chiralcel OD-H analytical column (250 × 4.6 mm) using n-hexane: ethanol (98:2, v/v) containing 0.2% triethylamine as mobile phase with a flow rate of 1.0 mL min-1 at 25°C. Online UV and optical rotation (OR) detection was performed at 254 nm. The parameters which have an effect on chiral separation were investigated, including mobile phase additive, organic modifier type and concentration, column temperature and flow rate. The method was tested for precision, accuracy, linearity, limit of detection (LOD), limit of quantification (LOQ) and robustness. The present method is expected to be accurate, stable, rapid and sensitive and can be used for the determination of the enantiomeric purity of 2-(aminomethyl)-1-ethylpyrrolidine in bulk samples.

【 授权许可】

Unknown