Simultaneous quantification of 28 synthetic cathinones and metabolites in urine by liquid chromatography-high resolution mass spectrometry

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• 作者：Marta Concheiro (1)
  Sebastien Anizan (1)
  Kayla Ellefsen (1)
  Marilyn A. Huestis (1)
  
• 关键词：Synthetic cathinones ; Urine ; LC ; HRMS ; Stability
• 刊名：Analytical and Bioanalytical Chemistry
• 出版年：2013
• 出版时间：November 2013
• 年：2013
• 卷：405
• 期：29
• 页码：9437-9448
• 全文大小：
• 作者单位：Marta Concheiro (1)
  Sebastien Anizan (1)
  Kayla Ellefsen (1)
  Marilyn A. Huestis (1)
  
  1. Chemistry and Drug Metabolism, Intramural Research Program, National Institute on Drug Abuse, National Institutes of Health, 251 Bayview Boulevard, Suite 200, Room 05A721, Baltimore, MD, 21224, USA
  
• ISSN：1618-2650

文摘

Synthetic cathinones are novel stimulants derived from cathinone, with amphetamines or cocaine-like effects, often labeled ot for human consumptionand considered egal highs Emergence of these new designer drugs complicate interpretation of forensic and clinical cases, with introduction of many new analogs designed to circumvent legislation and vary effects and potencies. We developed a method for the simultaneous quantification of 28 synthetic cathinones, including four metabolites, in urine by liquid chromatography coupled to high resolution mass spectrometry (LC-HRMS). These cathinones include cathinone, methcathinone, and synthetic cathinones position-3substituted, N-alkyl-substituted, ring-substituted, methylenedioxy-substituted, and pyrrolidinyl-substituted. One mL phosphate buffer pH6 and 25 IStd solution were combined with 0.25mL urine, and subjected to solid phase cation exchange extraction (SOLA SCX). The chromatographic reverse-phase separation was achieved with a gradient mobile phase of 0.1% formic acid in water and in acetonitrile in 20min. We employed a Q Exactive high resolution mass spectrometer, with compounds identified and quantified by target-MSMS experiments. The assay was linear from 0.5 to 100/L, with limits of detection of 0.25/L. Imprecision (n=20) was <15.9% and accuracy (n=20) 85.218.1%. Extraction efficiency was 78.916.7% (CV 1.46.7%, n=5), process efficiency 57.704.9%, and matrix effects from 29.5% to 1.5% (CV 1.93.1%, n=10). Most synthetic cathinones were stable at 4 for 72h (n=27) and after 3 freeze-thaw cycles (n=26), but many (n=19) were not stable at room temperature for 24h (losses up to 67.6%). The method was applied to authentic urine specimens from synthetic cathinone users. This method provides a comprehensive confirmation method for 28 synthetic cathinones in urine, with good selectivity and specificity.