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Liquid chromatography-atmospheric pressure ionization electrospray mass spectrometry determination of "hallucinogenic designer drugs" in urine of consumers.
J Pharm Biomed Anal. 2008 Jun 09; 47(2):335-42.JP

Abstract

A procedure based on liquid chromatography-mass spectrometry (LC-MS) is described for determination of 3,4-methylenedioxymethamphetamine (MDMA), 2,5-dimethoxy-4-methyl-phenethylamine (2C-D), 4-bromo-2,5-dimethoxy-beta-phenethylamine (2C-B), 1-(8-bromo-2,3,6,7-tetrahydrobenzo[1,2-b:4,5-b'] difuran-4-yl)-2-aminoethane (2C-B-Fly), 4-ethylthio-2,5-dimethoxy-beta-phenethylamine (2C-T-2), 4-iodo-2,5-dimethoxy-beta-phenethylamine (2C-I), and 4-ethyl-2,5-dimethoxy-beta-phenethylamine (2C-E), 1-(m-chlorophenyl)piperazine (m-CPP), 4-hydroxy-N,N-diisopropyltryptamine (4-OH-DIPT) and 4-acetoxy-N,N-diisopropyltryptamine (4-acetoxy-DIPT) in urine of consumers using 3,4 methylendioxypropylamphetamine (MDPA) as internal standard. Sample preparation involved a solid-phase extraction procedure at pH 6 of both non-hydrolyzed and enzymatically hydrolyzed urine samples. Chromatography was performed on a C(18) reversed-phase column using a linear gradient of 10mM ammonium bicarbonate, pH 7.3 and acetonitrile as a mobile phase. Separated analytes were determined in LC-MS single ion monitoring mode using an atmospheric pressure ionization-electrospray ionization (ESI) interface. The assay was tested on urine samples from consumers of compounds under investigation (n=32). Limits of quantification varied between 20 and 60 ng/mL for the different analytes under investigation. Calibration curves were linear to 2000 ng/mL for all the substances under investigation, with a minimum r(2)>0.99. At three concentrations spanning the linear dynamic range of the assay, mean recoveries ranged between 55.4 and 95.6% for the different analytes. Higher analytes concentrations in hydrolyzed samples showed the presence of conjugated compounds in urine.

Authors+Show Affiliations

Department of Therapeutic Research and Medicines Evaluation, Istituto Superiore di Sanità, Rome, Italy. simona.pichini@iss.itNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Comparative Study
Journal Article
Research Support, Non-U.S. Gov't

Language

eng

PubMed ID

18262381

Citation

Pichini, Simona, et al. "Liquid Chromatography-atmospheric Pressure Ionization Electrospray Mass Spectrometry Determination of "hallucinogenic Designer Drugs" in Urine of Consumers." Journal of Pharmaceutical and Biomedical Analysis, vol. 47, no. 2, 2008, pp. 335-42.
Pichini S, Pujadas M, Marchei E, et al. Liquid chromatography-atmospheric pressure ionization electrospray mass spectrometry determination of "hallucinogenic designer drugs" in urine of consumers. J Pharm Biomed Anal. 2008;47(2):335-42.
Pichini, S., Pujadas, M., Marchei, E., Pellegrini, M., Fiz, J., Pacifici, R., Zuccaro, P., Farré, M., & de la Torre, R. (2008). Liquid chromatography-atmospheric pressure ionization electrospray mass spectrometry determination of "hallucinogenic designer drugs" in urine of consumers. Journal of Pharmaceutical and Biomedical Analysis, 47(2), 335-42. https://doi.org/10.1016/j.jpba.2007.12.039
Pichini S, et al. Liquid Chromatography-atmospheric Pressure Ionization Electrospray Mass Spectrometry Determination of "hallucinogenic Designer Drugs" in Urine of Consumers. J Pharm Biomed Anal. 2008 Jun 9;47(2):335-42. PubMed PMID: 18262381.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Liquid chromatography-atmospheric pressure ionization electrospray mass spectrometry determination of "hallucinogenic designer drugs" in urine of consumers. AU - Pichini,Simona, AU - Pujadas,Mitona, AU - Marchei,Emilia, AU - Pellegrini,Manuela, AU - Fiz,Jimena, AU - Pacifici,Roberta, AU - Zuccaro,Piergiorgio, AU - Farré,Magi, AU - de la Torre,Rafael, Y1 - 2008/01/04/ PY - 2007/10/09/received PY - 2007/12/20/revised PY - 2007/12/21/accepted PY - 2008/2/12/pubmed PY - 2008/7/30/medline PY - 2008/2/12/entrez SP - 335 EP - 42 JF - Journal of pharmaceutical and biomedical analysis JO - J Pharm Biomed Anal VL - 47 IS - 2 N2 - A procedure based on liquid chromatography-mass spectrometry (LC-MS) is described for determination of 3,4-methylenedioxymethamphetamine (MDMA), 2,5-dimethoxy-4-methyl-phenethylamine (2C-D), 4-bromo-2,5-dimethoxy-beta-phenethylamine (2C-B), 1-(8-bromo-2,3,6,7-tetrahydrobenzo[1,2-b:4,5-b'] difuran-4-yl)-2-aminoethane (2C-B-Fly), 4-ethylthio-2,5-dimethoxy-beta-phenethylamine (2C-T-2), 4-iodo-2,5-dimethoxy-beta-phenethylamine (2C-I), and 4-ethyl-2,5-dimethoxy-beta-phenethylamine (2C-E), 1-(m-chlorophenyl)piperazine (m-CPP), 4-hydroxy-N,N-diisopropyltryptamine (4-OH-DIPT) and 4-acetoxy-N,N-diisopropyltryptamine (4-acetoxy-DIPT) in urine of consumers using 3,4 methylendioxypropylamphetamine (MDPA) as internal standard. Sample preparation involved a solid-phase extraction procedure at pH 6 of both non-hydrolyzed and enzymatically hydrolyzed urine samples. Chromatography was performed on a C(18) reversed-phase column using a linear gradient of 10mM ammonium bicarbonate, pH 7.3 and acetonitrile as a mobile phase. Separated analytes were determined in LC-MS single ion monitoring mode using an atmospheric pressure ionization-electrospray ionization (ESI) interface. The assay was tested on urine samples from consumers of compounds under investigation (n=32). Limits of quantification varied between 20 and 60 ng/mL for the different analytes under investigation. Calibration curves were linear to 2000 ng/mL for all the substances under investigation, with a minimum r(2)>0.99. At three concentrations spanning the linear dynamic range of the assay, mean recoveries ranged between 55.4 and 95.6% for the different analytes. Higher analytes concentrations in hydrolyzed samples showed the presence of conjugated compounds in urine. SN - 0731-7085 UR - https://www.unboundmedicine.com/medline/citation/18262381/Liquid_chromatography_atmospheric_pressure_ionization_electrospray_mass_spectrometry_determination_of_"hallucinogenic_designer_drugs"_in_urine_of_consumers_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0731-7085(08)00003-4 DB - PRIME DP - Unbound Medicine ER -