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Estimation of Enantiomeric Impurity in Piperidin‐3‐Amine by Chiral HPLC With Precolumn Derivatization
Author(s) -
Raghunadha Babu Chittabathina Venkata,
Vuyyuru Nagi Reddy,
Padmaja Reddy K.,
Suryanarayana M.V.,
Mukkanti K.
Publication year - 2014
Publication title -
chirality
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.43
H-Index - 77
eISSN - 1520-636X
pISSN - 0899-0042
DOI - 10.1002/chir.22352
Subject(s) - chemistry , chromatography , enantiomer , derivatization , amine gas treating , analyte , high performance liquid chromatography , chiral derivatizing agent , reagent , enantiomeric excess , toluene , benzoyl chloride , impurity , chiral column chromatography , organic chemistry , enantioselective synthesis , catalysis
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.