Chiral separation and determination of ketamine and norketamine in hair by capillary electrophoresis

Porpiglia, Nadia Maria; Musile, Giacomo; Bortolotti, Federica; Palo, Elio Franco De; Tagliaro, Franco

doi:10.1016/j.forsciint.2016.06.017

Cited by 32 publications

(25 citation statements)

References 32 publications

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“…Analytical methods which are based on enantioselective capillary electrophoresis were primarily developed to analyze ketamine, norketamine and DHNK . In the microassay of Theurillat et al.…”

Section: Introductionmentioning

confidence: 99%

Separation of hydroxynorketamine stereoisomers using capillary electrophoresis with sulfated β‐cyclodextrin and highly sulfated γ‐cyclodextrin

2017

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The racemic N-methyl-d-aspartate receptor antagonist ketamine is used in anesthesia, analgesia and the treatment of depressive disorders. It is known that interactions of hydroxylated norketamine metabolites and 5,6-dehydronorketamine (DHNK) with the α -nicotinic acetylcholine receptor and the α-amino-3-hydroxy-5-methyl-4-isoxazolepropionic acid receptor are responsible for the antidepressive effects. Ketamine and its first metabolite norketamine are not active on these receptors. As stereoselectivity plays a role in ketamine metabolism, a cationic capillary electrophoresis based method capable of resolving and analyzing the stereoisomers of four hydroxylated norketamine metabolites, norketamine and DHNK was developed. The assay is based on liquid/liquid extraction of the analytes from the biological matrix, electrokinetic sample injection across a buffer plug and analysis of the stereoisomers in a phosphate background electrolyte (BGE) at pH 3 comprising a mixture of sulfated β-cyclodextrin (5 mg/mL) and highly sulfated γ-cyclodextrin (0.1%). The method was used to analyze samples of an in vitro study in which ketamine was incubated with equine liver microsomes and in plasma samples of dogs and horses that were collected after an i.v. bolus injection of racemic ketamine.

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Section: Introductionmentioning

confidence: 99%

Separation of hydroxynorketamine stereoisomers using capillary electrophoresis with sulfated β‐cyclodextrin and highly sulfated γ‐cyclodextrin

2017

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“…Key parameters for optimization of the FASI injection were identified as being the length of the buffer plug and its concentration, and the voltage and time for the electrokinetic injection. Under optimized conditions (described in Table ), on the one hand, ketamine and norketamine enantiomers in hair samples were detected with an LOD of 80 ppb , and, on the other hand, it was possible to detect the enantiomers of ketamine and three of its major metabolites in plasma or serum with an LOD of only 3 ppb . Typical electropherograms obtained from dog plasma samples are presented in Fig.…”

Section: Strategies To Improve the Detection Sensitivitymentioning

confidence: 99%

“…Under these conditions, LODs of 0.9 parts per million (ppm) were achieved. LLE has also been used in the extraction of ketamine and its metabolites from hair or biological fluids , methorphan and its metabolites from blood , propranolol from biological fluids , and methamphetamine from hair . These last works, in addition to using LLE, also employ an in‐capillary sample preconcentration technique to improve the sensitivity of the chiral separations obtained (see Table ) and are described in Section .…”

Section: Strategies To Improve the Detection Sensitivitymentioning

confidence: 99%

“…Ketamine and its metabolites extracted previously with LLE of hair samples or biological fluids have been preconcentrated by means of FASI in an EKC‐UV system. In both cases, a short plug of the running buffer or a diluted buffer without the chiral selector (a negatively charged CD) was hydrodynamically injected to create a zone of lower conductivity.…”

Section: Strategies To Improve the Detection Sensitivitymentioning

confidence: 99%

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Recent contributions for improving sensitivity in chiral CE

2017

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The flexibility and versatility of the chiral CE are unrivaled and the same instrumentation can be used to separate a diverse range of analytes, both large and small molecules, whether charged or uncharged. However, one of the disadvantages is generally thought to be the poor sensitivity of ultraviolet (UV) detection, which is the most popular among CE detectors. This review focuses on methodologies and applications regarding improvements of sensitivity in chiral CE published in the last 2 years (June 2015 until May 2017). This contribution continues to update this series of biannual reviews, first published in Electrophoresis in 2006. The main body of the review brings a survey of publications organized according to different approaches to detect a low amount of analytes, either by sample treatment procedures or by in-capillary sample preconcentration techniques, both using UV detection, or even by employing detection systems more sensitive than UV absorption, such as LIF or MS. This review provides comprehensive tables listing the new approaches in sensitive chiral CE with categorizing by the fundamental mechanism to enhance the sensitivity, which provide relevant information on the strategies employed. The concluding remarks in the final part of the review evaluate present state of art and the trends for sensitivity enhancement in chiral CE.

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“…In fact, K can be bought in the internet from suspected veterinary distributers and clinics [ 109 ]. Chiral discrimination of K and its main metabolite norketamine (NK) was done in in plasma and hair [ 110 , 111 ]. S -(+)-K is an anesthetic and analgesic but R -(−)-ketamine is associated to hallucinations and agitation.…”

Section: Chiral Analyses In Biological Samplesmentioning

confidence: 99%

Chiral Drug Analysis in Forensic Chemistry: An Overview

et al. 2018

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Many substances of forensic interest are chiral and available either as racemates or pure enantiomers. Application of chiral analysis in biological samples can be useful for the determination of legal or illicit drugs consumption or interpretation of unexpected toxicological effects. Chiral substances can also be found in environmental samples and revealed to be useful for determination of community drug usage (sewage epidemiology), identification of illicit drug manufacturing locations, illegal discharge of sewage and in environmental risk assessment. Thus, the purpose of this paper is to provide an overview of the application of chiral analysis in biological and environmental samples and their relevance in the forensic field. Most frequently analytical methods used to quantify the enantiomers are liquid and gas chromatography using both indirect, with enantiomerically pure derivatizing reagents, and direct methods recurring to chiral stationary phases.

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Chiral separation and determination of ketamine and norketamine in hair by capillary electrophoresis

Cited by 32 publications

References 32 publications

Separation of hydroxynorketamine stereoisomers using capillary electrophoresis with sulfated β‐cyclodextrin and highly sulfated γ‐cyclodextrin

Separation of hydroxynorketamine stereoisomers using capillary electrophoresis with sulfated β‐cyclodextrin and highly sulfated γ‐cyclodextrin

Recent contributions for improving sensitivity in chiral CE

Chiral Drug Analysis in Forensic Chemistry: An Overview

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