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Vol. 25 No. 3 (2013): Vol 25 Issue 3

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Determination of Enantiomeric Purity of 2-Piperidinemethanamine by HPLC Combined With Pre-Column Derivation

https://doi.org/10.14233/ajchem.2013.12992
Yi-Wen Zhang
Department of Pharmaceutical and Biological Engineering, School of Chemical Engineering, Sichuan University, Chengdu 610065, P.R. China
Ji Luo
Department of Pharmaceutical and Biological Engineering, School of Chemical Engineering, Sichuan University, Chengdu 610065, P.R. China
Hao Zeng
Department of Pharmaceutical and Biological Engineering, School of Chemical Engineering, Sichuan University, Chengdu 610065, P.R. China
Shun Yao
Department of Pharmaceutical and Biological Engineering, School of Chemical Engineering, Sichuan University, Chengdu 610065, P.R. China
Hao Chen
Department of Pharmaceutical and Biological Engineering, School of Chemical Engineering, Sichuan University, Chengdu 610065, P.R. China
Hang Song
Department of Pharmaceutical and Biological Engineering, School of Chemical Engineering, Sichuan University, Chengdu 610065, P.R. China

Corresponding Author(s) : Hang Song

hangsong@scu.edu.cn

Asian Journal of Chemistry, Vol. 25 No. 3 (2013): Vol 25 Issue 3

Abstract

A new HPLC method has been developed and validated for determination of enantiomeric purity of 2-piperidinemethanamine within a short run time of less than 10 min. The method was based on pre-column derivation of 2-piperidinemethanamine with 3,5-dinitrobenzoic acid and complete separation of enantiomers has been achieved on a CHI-DMB analytical column (250 mm × 4.6 mm) using n-hexane: ethanol (85:15 v/v) as mobile phase at a flow rate of 1.0 mL min-1 under UV photodiode-array detector detection. Then the effects of mobile phase and temperature on enantioselectivity were further evaluated. The method was validated with respect to precision, accuracy, linearity, limit of detection (LOD), limit of quantification (LOQ) and robustness. The recoveries were between 99.1 and 102.3 % with percentage relative standard deviation less than 1.17 %. The LOD and LOQ for first enantiomer were 13.7 and 46.3 μg mL-1 and for second enantiomer were 15.2 and 51.4 μg mL-1, respectively. This method is expected to be accurate, stable, rapid and sensitive for determination of the enantiomeric purity of 2-piperidinemethanamine in bulk samples.

Keywords

Liquid chromatography Enantiomeric purity 2-Piperidinemethanamine Pre-column derivation Method validation
Zhang, Y.-W., Luo, J., Zeng, H., Yao, S., Chen, H., & Song, H. (2012). Determination of Enantiomeric Purity of 2-Piperidinemethanamine by HPLC Combined With Pre-Column Derivation. Asian Journal of Chemistry, 25(3), 1353–1356. https://doi.org/10.14233/ajchem.2013.12992
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