A rapid method for the extraction, enantiomeric separation and quantification of amphetamines in hair

Rossi, Sabina Strano; Botrè, Francesco; Bermejo, Ana María; Tabernero, María Jesús

doi:10.1016/j.forsciint.2009.09.016

Cited by 33 publications

(24 citation statements)

References 27 publications

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“…1, who was a CYP2D6 poor metabolizer, had the highest R/S-MDMA ratio in the hair segment corresponding to the time of intake and the nail scraping whereas the ratio in the nail clipping was in the range of the extensive CYP2D6 metabolizers ( Figure 3A). To our knowledge, there are two reports on chiral analysis of MDMA and MDA in hair samples from suspected or self-declared MDMA users [41][42][43]. Enantiomeric ratios for MDMA and MDA from our controlled intake study are in concordance with hair findings reported by Martins et al from a study with self-declared MDMA users after controlled MDMA administration [41].…”

Section: Mdma and Mda In Nail Samples And Comparison To Hairsupporting

confidence: 90%

Evaluation of drug incorporation into hair segments and nails by enantiomeric analysis following controlled single MDMA intakes

et al. 2015

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Incorporation rates of the enantiomers of 3,4-methylenedioxymethamphetamine (MDMA) and its metabolite 3,4-methylenedioxyamphetamine (MDA) into hair and nails were investigated after controlled administration. Fifteen subjects without MDMA use received two doses of 125 mg of MDMA. Hair, nail scrapings and nail clippings were collected 9-77 days after the last administration (median: 20 days).Hair samples were analyzed in segments of 1-to 2-cm length. After chiral derivatization with N-(2,4-dinitro-5-fluorophenyl)-L-valinamide, MDMA and MDA diastereomers were analyzed by liquid chromatography-tandem mass spectrometry.Highest concentrations in hair segments corresponded to the time of MDMA intake.

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Section: Mdma and Mda In Nail Samples And Comparison To Hairsupporting

confidence: 90%

Evaluation of drug incorporation into hair segments and nails by enantiomeric analysis following controlled single MDMA intakes

et al. 2015

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“…(S)-TFPC has been utilized as CDR for enantiomeric resolution of amphetamine and methamphetamine in biological fluids such as urine and blood [10][11][12], and hair [13] by gas chromatography-mass spectroscopy. Camphanic chloride has been utilized to synthesize diastereomers of different alcohols [14][15][16][17]; the diastereomers, so formed, were separated by column chromatography and were hydrolyzed to individual enantiomers.…”

Section: Fig 1 Synthesis Of Diastereomers Of (R S)-mex Using (S)-(mentioning

confidence: 99%

High-performance liquid chromatography for analytical and small-scale preparative separation of (R,S)-mexiletine using (S)-(—)-(N)-trifluoroacetyl-prolyl chloride and (1S)-(—)-camphanic chloride and recovery of native enantiomer by detagging

Dixit¹,

Dubey²,

Bhushan³

2014

Acta Chromatographica

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Summary.A reversed phase high-performance liquid chromatographic method has been established for enantioseparation of (R, S)-mexiletine. Two volatile and thermally stable acyl chlorides, viz., (S)-(−)-(N)-trifluoro acetyl prolyl chloride and (1S)-(−)-camphanic chloride, were used as chiral derivatizing reagents. Binary composition of aqueous trifluoroacetic acid (0.1%)-acetonitrile as mobile phase was successful with ultraviolet (UV) detection at 210 nm. The method was optimized and validated for accuracy, precision, and limit of detection. The limit of detection was found to be 45 ng mL −1 and 80 ng mL −1 for the two types of diastereomers. Besides, kinetic resolution was achieved, and the experimental conditions optimized for this purpose provided diastereomeric excess up to 74% for (R)-isomer. On achieving a resolution value greater than 2, the optimized method for analytical enantioseparation was scaled-up to smallscale preparative level, and the native (R)-mexiletine was recovered by acid hydrolysis of the diastereomer.

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“…The first one is pre-column derivatization with a chiral derivatization reagent to generate diastereomers; the second one involves adding a chiral agent to the mobile phase to form adducts with the enantiomers; and the third one is a direct method using chiral stationary phase [20] [25]. GC methods involve complicated and time consuming pre-column derivatization steps [3] [8] [12]- [14]. Liquid chromatography mass spectrometry (LC-MS) has gained more and more popularity for drug analysis because it is generally faster, easy to use and has better sensitivity and specificity [22] [23].…”

Section: Introductionmentioning

confidence: 99%

Fast and Sensitive Chiral Analysis of Amphetamines and Cathinones in Equine Urine and Plasma Using Liquid Chromatography Tandem Mass Spectrometry

Wang

Hartmann-Fischbach

Krueger

et al. 2015

AJAC

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A simple, rapid, sensitive and reproducible method for enantiomer analysis of methamphetamine, amphetamine, cathinone and methcathinone was developed and validated. The compounds were extracted from equine plasma and urine using a fast liquid-liquid extraction procedure. Only one milliliter plasma and one hundred microliter urine sample is needed for analysis. The extraction procedure had good recovery (>70%) and the matrix effect was negligible. Enantiomer differentiation and confirmation were achieved using liquid chromatography with chiral stationary phase and mass spectrometry detection. The method demonstrated excellent reproducibility with intraday and inter-day precision of lower than 5%. The lower limits of detection for all of the compounds studied here were at low pg/mL level for both plasma and urine. This is the first report of the analysis of four chiral compounds in equine plasma and urine. Routine application was demonstrated for (S)-and (R)-enantiomer differentiation.

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A rapid method for the extraction, enantiomeric separation and quantification of amphetamines in hair

Cited by 33 publications

References 27 publications

Evaluation of drug incorporation into hair segments and nails by enantiomeric analysis following controlled single MDMA intakes

Evaluation of drug incorporation into hair segments and nails by enantiomeric analysis following controlled single MDMA intakes

High-performance liquid chromatography for analytical and small-scale preparative separation of (R,S)-mexiletine using (S)-(—)-(N)-trifluoroacetyl-prolyl chloride and (1S)-(—)-camphanic chloride and recovery of native enantiomer by detagging

Fast and Sensitive Chiral Analysis of Amphetamines and Cathinones in Equine Urine and Plasma Using Liquid Chromatography Tandem Mass Spectrometry

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