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Simultaneous quantification of 28 synthetic cathinones and metabolites in urine by liquid chromatography-high resolution mass spectrometry.
Anal Bioanal Chem. 2013 Nov; 405(29):9437-48.AB

Abstract

Synthetic cathinones are novel stimulants derived from cathinone, with amphetamines or cocaine-like effects, often labeled "not for human consumption" and considered "legal 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-3'-substituted, N-alkyl-substituted, ring-substituted, methylenedioxy-substituted, and pyrrolidinyl-substituted. One mL phosphate buffer pH 6 and 25 μL IStd solution were combined with 0.25 mL 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 20 min. We employed a Q Exactive high resolution mass spectrometer, with compounds identified and quantified by target-MSMS experiments. The assay was linear from 0.5-1 to 100 μg/L, with limits of detection of 0.25-1 μg/L. Imprecision (n = 20) was <15.9 % and accuracy (n = 20) 85.2-118.1 %. Extraction efficiency was 78.9-116.7 % (CV 1.4-16.7 %, n = 5), process efficiency 57.7-104.9 %, and matrix effects from -29.5 % to 1.5 % (CV 1.9-13.1 %, n = 10). Most synthetic cathinones were stable at 4 °C for 72 h (n = 27) and after 3 freeze-thaw cycles (n = 26), but many (n = 19) were not stable at room temperature for 24 h (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.

Authors+Show Affiliations

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.No affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Evaluation Study
Journal Article
Research Support, N.I.H., Intramural

Language

eng

PubMed ID

24196122

Citation

Concheiro, Marta, et al. "Simultaneous Quantification of 28 Synthetic Cathinones and Metabolites in Urine By Liquid Chromatography-high Resolution Mass Spectrometry." Analytical and Bioanalytical Chemistry, vol. 405, no. 29, 2013, pp. 9437-48.
Concheiro M, Anizan S, Ellefsen K, et al. Simultaneous quantification of 28 synthetic cathinones and metabolites in urine by liquid chromatography-high resolution mass spectrometry. Anal Bioanal Chem. 2013;405(29):9437-48.
Concheiro, M., Anizan, S., Ellefsen, K., & Huestis, M. A. (2013). Simultaneous quantification of 28 synthetic cathinones and metabolites in urine by liquid chromatography-high resolution mass spectrometry. Analytical and Bioanalytical Chemistry, 405(29), 9437-48. https://doi.org/10.1007/s00216-013-7386-z
Concheiro M, et al. Simultaneous Quantification of 28 Synthetic Cathinones and Metabolites in Urine By Liquid Chromatography-high Resolution Mass Spectrometry. Anal Bioanal Chem. 2013;405(29):9437-48. PubMed PMID: 24196122.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Simultaneous quantification of 28 synthetic cathinones and metabolites in urine by liquid chromatography-high resolution mass spectrometry. AU - Concheiro,Marta, AU - Anizan,Sebastien, AU - Ellefsen,Kayla, AU - Huestis,Marilyn A, Y1 - 2013/10/03/ PY - 2013/08/07/received PY - 2013/09/16/accepted PY - 2013/09/12/revised PY - 2013/11/8/entrez PY - 2013/11/8/pubmed PY - 2014/6/16/medline SP - 9437 EP - 48 JF - Analytical and bioanalytical chemistry JO - Anal Bioanal Chem VL - 405 IS - 29 N2 - Synthetic cathinones are novel stimulants derived from cathinone, with amphetamines or cocaine-like effects, often labeled "not for human consumption" and considered "legal 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-3'-substituted, N-alkyl-substituted, ring-substituted, methylenedioxy-substituted, and pyrrolidinyl-substituted. One mL phosphate buffer pH 6 and 25 μL IStd solution were combined with 0.25 mL 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 20 min. We employed a Q Exactive high resolution mass spectrometer, with compounds identified and quantified by target-MSMS experiments. The assay was linear from 0.5-1 to 100 μg/L, with limits of detection of 0.25-1 μg/L. Imprecision (n = 20) was <15.9 % and accuracy (n = 20) 85.2-118.1 %. Extraction efficiency was 78.9-116.7 % (CV 1.4-16.7 %, n = 5), process efficiency 57.7-104.9 %, and matrix effects from -29.5 % to 1.5 % (CV 1.9-13.1 %, n = 10). Most synthetic cathinones were stable at 4 °C for 72 h (n = 27) and after 3 freeze-thaw cycles (n = 26), but many (n = 19) were not stable at room temperature for 24 h (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. SN - 1618-2650 UR - https://www.unboundmedicine.com/medline/citation/24196122/Simultaneous_quantification_of_28_synthetic_cathinones_and_metabolites_in_urine_by_liquid_chromatography_high_resolution_mass_spectrometry_ L2 - https://dx.doi.org/10.1007/s00216-013-7386-z DB - PRIME DP - Unbound Medicine ER -