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Chirality2020; 32(3); 314-323; doi: 10.1002/chir.23166

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.

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.
© 2020 Wiley Periodicals, Inc.
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Publication Date: 2020-01-10 PubMed ID: 31925851DOI: 10.1002/chir.23166Google Scholar: Lookup
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  • Journal Article
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Summary

This research summary has been generated with artificial intelligence and may contain errors and omissions. Refer to the original study to confirm details provided. Submit correction.

This research article focuses on devising a simpler and more efficient method for the detection and separation of medetomidine enantiomers in equine plasma using a polysaccharide cellulose chiral column, specifically the chiralcel OJ-3R. The new method proves to be accurate and efficient, offering potential for routine analysis in forensic toxicology and pharmacology.

Background

  • The primary challenges highlighted in the paper are the detection and separation of medetomidine enantiomers from complex biological matrices. These challenges are particularly relevant in forensic toxicology and pharmacology.
  • Previous research had attempted to resolve medetomidine using protein-based chiral columns, but these methods were found to be difficult and cumbersome for regular use.

Methodology

  • The researchers introduced a new method for separating medetomidine enantiomers using a polysaccharide cellulose chiral column.
  • The chiralcel OJ-3R column demonstrated the most potential for successful chiral resolution out of the various columns tested.
  • Ammonium hydrogen carbonate was found to be the optimal buffer salt for chiral liquid chromatography (LC), with electrospray ionization (ESI)+ mass spectrometry (MS) detection enabling the successful separation and detection of the racemic compound.

Results and Analysis

  • The method proved linear over a range of 0 to 20 ng/mL in equine plasma with the inter-day precisions of levomedetomidine and dexmedetomidine at 1.36% and 1.89%, respectively.
  • Accuracy rates were high: levomedetomidine ranged from 99.25% to 101.57%, while dexmedetomidine ranged from 99.17% to 100.99%.
  • The limits of quantification for both isomers were 0.2 ng/mL, illustrating high precision.
  • Recovery and the matrix effect on the analytes were also evaluated and factored into the overall assessment of the method’s efficacy.

Conclusion

  • Under the optimized conditions, the new method is valid for the identification and resolution of the medetomidine enantiomers in various matrices used for drug testing and analysis.
  • This modified method allows for more straightforward and routine analysis, which was previously a challenge with protein-based chiral columns.

Cite This Article

APA
Karakka Kal AK, Nalakath J, Kunhamu Karatt T, Perwad Z, Mathew B, Subhahar M. (2020). 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. Chirality, 32(3), 314-323. https://doi.org/10.1002/chir.23166

Publication

Chirality
ISSN: 1520-636X
NlmUniqueID: 8914261
Country: United States
Language: English
Volume: 32
Issue: 3
Pages: 314-323

Researcher Affiliations

Karakka Kal, Abdul Khader
  • Equine Forensic Unit, Central Veterinary Research Laboratory, Dubai, United Arab Emirates.
Nalakath, Jahfar
  • Equine Forensic Unit, Central Veterinary Research Laboratory, Dubai, United Arab Emirates.
Kunhamu Karatt, Tajudheen
  • Equine Forensic Unit, Central Veterinary Research Laboratory, Dubai, United Arab Emirates.
Perwad, Zubair
  • Equine Forensic Unit, Central Veterinary Research Laboratory, Dubai, United Arab Emirates.
Mathew, Binoy
  • Equine Forensic Unit, Central Veterinary Research Laboratory, Dubai, United Arab Emirates.
Subhahar, Michael
  • Equine Forensic Unit, Central Veterinary Research Laboratory, Dubai, United Arab Emirates.

MeSH Terms

  • Animals
  • Cellulose / chemistry
  • Chromatography, Liquid / methods
  • Dexmedetomidine / blood
  • Dexmedetomidine / isolation & purification
  • Horses
  • Limit of Detection
  • Medetomidine / blood
  • Medetomidine / chemistry
  • Medetomidine / isolation & purification
  • Spectrometry, Mass, Electrospray Ionization / methods
  • Stereoisomerism

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Citations

This article has been cited 2 times.
  1. Bui CV, Rosenau T, Hettegger H. Polysaccharide- and β-Cyclodextrin-Based Chiral Selectors for Enantiomer Resolution: Recent Developments and Applications. Molecules 2021 Jul 16;26(14).
    doi: 10.3390/molecules26144322pubmed: 34299597google scholar: lookup
  2. Karakka Kal AK, Karatt TK, Nalakath J, Subhahar MB, Koshy SA, Perwad Z, M P MA. Simultaneous analysis of 44 frequently abused corticosteroid drugs using polysaccharide-based chiral column-HRMS approach. Anal Sci Adv 2021 Oct;2(9-10):427-439.
    doi: 10.1002/ansa.202000166pubmed: 38716441google scholar: lookup
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