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Development and validation of a chiral LC‐MS method for the enantiomeric resolution of (+) and (−)‐medetomidine in equine plasma by using polysaccharide‐based chiral stationary phases
Author(s) -
Karakka Kal Abdul Khader,
Nalakath Jahfar,
Kunhamu Karatt Tajudheen,
Perwad Zubair,
Mathew Binoy,
Subhahar Michael
Publication year - 2020
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.23166
Subject(s) - chemistry , medetomidine , enantiomer , chromatography , analyte , electrospray ionization , resolution (logic) , electrospray , detection limit , mass spectrometry , cellulose , stereochemistry , organic chemistry , medicine , heart rate , artificial intelligence , computer science , blood pressure , radiology
Abstract The detection and separation of medetomidine enantiomers from the complex biological matrices poses a great analytical challenge, especially in the field of forensic toxicology and pharmacology. Couple of researchers reported resolution of medetomidine using protein‐based chiral columns, but the reported method is quiet challenging and tedious to be employed for routine analysis. This research paper reported a method that enables the enantio‐separation of medetomidine by using polysaccharide cellulose chiral column. The use of chiralcel OJ‐3R column was found to have the highest potential for successful chiral resolution. Ammonium hydrogen carbonate was the ideal buffer salt for chiral liquid chromatography (LC) with electrospray ionization (ESI)+ mass spectrometry (MS) detection for the successful separation and detection of racemic compound. The method was linear over the range of 0 to 20 ng/mL in equine plasma and the inter‐day precisions of levomedetomidine, dexmedetomidine were 1.36% and 1.89%, respectively. The accuracy of levomedetomidine was in the range of 99.25% to 101.57% and that for dexmedetomidine was 99.17% to 100.99%. The limits of quantification for both isomers were 0.2 ng/mL. Recovery and matrix effect on the analytes were also evaluated. Under the optimized conditions, the validated method can be adapted for the identification and resolution of the medetomidine enantiomers in different matrices used for drug testing and analysis.