Analytical Sciences

Abstract − Analytical Sciences, 33(3), 293 (2017).

Fast and Simple Determination of 3-Aminopiperidine without Derivatization Using High Performance Liquid Chromatography–Charged Aerosol Detector with an Ion-Exchange/Reversed-Phase Mixed-mode Column
Shubo DONG,* Zhengyu YAN,* Hanyue YANG,** and Zhen LONG***
*China Pharmaceutical University, Longmian Road 639, Jiangning District, Nanjing 210000, Jiangsu, P. R. China
**Jiangsu Deyuan Pharmaceutical Co., Ltd, Jinqiao Road 21, Lianyungang 222002, Jiangsu, P. R. China
***Thermo Fisher Scientific Co., Ltd, Andingmen Road 28, Beijing 100000, P. R. China
A sensitive non-derivatization method for the determination of the highly polar compound 3-aminopiperidine was developed using a mixed-mode column combined with a charged aerosol detector (CAD). Chromatographic conditions, including the type of detector, separation mode, and mobile phase composition, were optimized to achieve high sensitivity towards and sufficient retention of 3-aminopiperidine. Compared to the precolumn derivatization UV method, the current method showed higher recovery and greater simplicify. High sensitivity (LOQ <2.73 μg mL−1) and good precision (RSD of peak area <2%) were also observed in the current method. Furthermore, the parameters such as buffer solution and column bleed that affected the sensitivity of the CAD were investigated. Finally, the current method was applied for the determination of 3-aminopiperidine in linagliptin samples. This is a new non-derivative for the determination of 3-aminopiperidine, and constitutes a novel application of the CAD for the quantitative analysis of highly polar basic compounds.