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| Content Provider | World Health Organization (WHO)-Global Index Medicus |
|---|---|
| Author | Concheiro, Marta Newmeyer, Matthew N. Huestis, Marilyn A. |
| Description | Country affiliation: United States Author Affiliation: Newmeyer MN ( Chemistry and Drug Metabolism Section, IRP, National Institute on Drug Abuse, National Institutes of Health, Baltimore, MD, USA); Concheiro M ( Chemistry and Drug Metabolism Section, IRP, National Institute on Drug Abuse, National Institutes of Health, Baltimore, MD, USA.); Huestis MA ( Chemistry and Drug Metabolism Section, IRP, National Institute on Drug Abuse, National Institutes of Health, Baltimore, MD, USA. Electronic address: mhuestis@intra.nida.nih.gov.) |
| Abstract | Methamphetamine is a widely abused psychostimulant containing a chiral center. Consumption of over-the-counter and prescription medications may yield positive amphetamines results, but chiral separation of l- and d-methamphetamine and its metabolite amphetamine can help determine whether the source was licit or illicit. We present the first LC-MS/MS method with precolumn derivatization for methamphetamine and amphetamine chiral resolution in plasma and oral fluid collected with the Oral-Eze(®) and Quantisal™ devices. To 0.5mL plasma, 0.75mL Oral-Eze, or 1mL Quantisal specimen racemic d11-methamphetamine and amphetamine internal standards were added, followed by protein precipitation. Samples were centrifuged and supernatants loaded onto pre-conditioned Phenomenex(®) Strata™-XC Polymeric Strong Cation solid phase extraction columns. After washing, analytes were eluted with 5% ammonium hydroxide in methanol. The eluate was evaporated to dryness and reconstituted in water. Derivatization was performed with 1-fluoro-2,4-dinitrophenyl-5-l-alanineamide (Marfey's reagent) and heating at 45°C for 1h. Derivatized enantiomer separations were performed under isocratic conditions (methanol:water, 60:40) with a Phenomenex(®) Kinetex(®) 2.6µm C18 column. Analytes were identified and quantified by two MRM transitions and their ratio on a 3200 QTrap (AB Sciex) mass spectrometer in ESI negative mode. In all three matrices, the method was linear for all enantiomers from 1 to 500µg/L, with imprecision and accuracy of ≤11.3% and 85.3-108%, respectively. Extraction efficiencies ranged from 67.4 to 117% and matrix effects from -17.0 to 468%, with variation always ≤19.1%. Authentic plasma and OF specimens were collected from an IRB-approved study that included controlled Vicks(®) VapoInhaler™ administration. The present method is sensitive, selective, economic and rapid (separations accomplished in <10min), and improves methamphetamine result interpretation. |
| ISSN | 00219673 |
| e-ISSN | 18733778 |
| DOI | 10.1016/j.chroma.2014.06.096 |
| Journal | Journal of Chromatography A |
| Volume Number | 1358 |
| Language | English |
| Publisher | Elsevier |
| Publisher Date | 2014-09-05 |
| Publisher Place | Netherlands |
| Access Restriction | Open |
| Subject Keyword | Alanine Analogs & Derivatives Central Nervous System Stimulants Isolation & Purification Dinitrobenzenes Chemistry Methamphetamine Blood Chromatography, High Pressure Liquid Limit Of Detection Reference Standards Saliva Spectrometry, Mass, Electrospray Ionization Stereoisomerism Tandem Mass Spectrometry Research Support, N.i.h., Intramural Research Support, U.s. Gov't, P.h.s. Discipline Analytical Chemistry |
| Content Type | Text |
| Resource Type | Article |
| Subject | Organic Chemistry Medicine Analytical Chemistry Biochemistry |
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