Estimation of Enantiomeric Impurity in Piperidin-3-Amine by Chiral HPLC With Precolumn Derivatization

• Published in: Chirality (New York, N.Y.) Vol. 26; no. 12; pp. 775 - 779
• Main Authors: Raghunadha Babu, Chittabathina Venkata, Vuyyuru, Nagi Reddy, Padmaja Reddy, K., Suryanarayana, M.V., Mukkanti, K.
• Format: Journal Article
• Language: English
• Published: United States Blackwell Publishing Ltd 01.12.2014; Wiley Subscription Services, Inc
• Subjects: Chirality; Chlorides; Chromatography, High Pressure Liquid - instrumentation; Chromatography, High Pressure Liquid - methods; Conferences; enantiomers; Ethyl alcohol; Guidelines; ICH; Limit of Detection; Liquids; Piperidines - analysis; Piperidines - chemistry; polar mode; PTSC; Reproducibility of Results; Solutions; Stereoisomerism; Tasks; Toluene; validation; PTSC; polar mode; enantiomers; validation; ICH
• ISSN: 0899-0042; 1520-636X
• DOI: 10.1002/chir.22352

ABSTRACT A simple, precise, accurate, robust chiral high‐performance liquid chromatographic (chiral HPLC) method was developed for estimation of (S)‐piperidin‐3‐amine (S‐isomer) in (R)‐piperidin‐3‐amine dihydrochloride (R‐AMP). As AMP is a high‐melting solid and nonchromophoric compound, development of a suitable chiral method is a challenging task. The proposed chiral HPLC‐UV method involves a precolumn derivatization technique with para toluene sulphonyl chloride (PTSC) in the presence of a base to introduce chromophore into analytes. It utilizes chiralpak AD‐H column with a simple mobile phase of 0.1% diethyl amine in ethanol with a 0.5 mL/min flow rate. Analytes were monitored by using a UV detector at 228 nm. The resolution between the two enantiomers was more than 4.0. The developed method was validated as per current International Conference on Harmonization (ICH) guidelines. Chirality 26:775–779, 2014. © 2014 Wiley Periodicals, Inc.