title: Estimation of enantiomeric impurity in piperidin-3-amine by chiral HPLC with precolumn derivatization.
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.
authors.affiliation: Dr. Reddy's Laboratories Ltd. IPDO, Bachupally, Hyderabad, A.P, India; Center for Pharmaceutical Sciences, IST, J.N.T.University, Kukatpally, Hyderabad, A.P, India.
authors.forename: Chittabathina Venkata
authors.initials: CV
authors.lastname: Raghunadha Babu
authors.forename: Nagi Reddy
authors.initials: NR
authors.lastname: Vuyyuru
authors.forename: K
authors.initials: K
authors.lastname: Padmaja Reddy
authors.forename: M V
authors.initials: MV
authors.lastname: Suryanarayana
authors.forename: K
authors.initials: K
authors.lastname: Mukkanti
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000295:instrumentation / Q000379:methods*; D057230:Limit of Detection; D010880:Piperidines / Q000032:analysis / Q000737:chemistry*; D015203:Reproducibility of Results; D012996:Solutions; D013237:Stereoisomerism
chemical_list: D010880:Piperidines; D012996:Solutions; C000599983:piperidin-3-amine
keywords: ICH; PTSC; enantiomers; polar mode; validation