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Analysis of phenylpiperazine-like stimulants in human hair as trimethylsilyl derivatives by gas chromatography-mass spectrometry.
J Chromatogr A. 2010 Oct 01; 1217(40):6274-80.JC

Abstract

A simple and sensitive procedure, using p-tolylpiperazine (pTP) as internal standard (IS), has been developed and validated for the qualitative and quantitative analysis of 1-(3-trifuoromethylphenyl)piperazine (TFMPP), 1-(3-chlorophenyl)piperazine (mCPP) and 1-(4-methoxyphenyl)piperazine (MeOPP) in hair. Drug extraction was performed by incubation with 1 M sodium hydroxide at 50°C for 40 min, and the extracts were cleaned up using mixed-mode solid-phase extraction. The analytes were derivatized with N-methyl-N-(trimethylsilyl) trifluoroacetamide with 5% trimethylchlorosilane and analysed by gas chromatography-mass spectrometry in the selected ion monitoring mode. The method was linear from 0.05 (lower limit of quantitation) to 4 ng mg(-1), with correlation coefficients higher than 0.99 for all the compounds. Intra- and interday precision and accuracy were in conformity with the criteria normally accepted in bioanalytical method validation, and the sample cleanup step presented a mean efficiency higher than 90% for all the analytes. Due to its simplicity and speed, this method can be successfully applied in the screening and quantitation of these compounds in hair samples, and is suitable for application in forensic toxicology routine analysis.

Authors+Show Affiliations

Instituto Nacional de Medicina Legal-Delegação do Sul, Rua Manuel Bento de Sousa, 3, 1150-219 Lisboa, Portugal. mbarroso@dlinml.mj.ptNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article

Language

eng

PubMed ID

20800845

Citation

Barroso, M, et al. "Analysis of Phenylpiperazine-like Stimulants in Human Hair as Trimethylsilyl Derivatives By Gas Chromatography-mass Spectrometry." Journal of Chromatography. A, vol. 1217, no. 40, 2010, pp. 6274-80.
Barroso M, Costa S, Dias M, et al. Analysis of phenylpiperazine-like stimulants in human hair as trimethylsilyl derivatives by gas chromatography-mass spectrometry. J Chromatogr A. 2010;1217(40):6274-80.
Barroso, M., Costa, S., Dias, M., Vieira, D. N., Queiroz, J. A., & López-Rivadulla, M. (2010). Analysis of phenylpiperazine-like stimulants in human hair as trimethylsilyl derivatives by gas chromatography-mass spectrometry. Journal of Chromatography. A, 1217(40), 6274-80. https://doi.org/10.1016/j.chroma.2010.08.001
Barroso M, et al. Analysis of Phenylpiperazine-like Stimulants in Human Hair as Trimethylsilyl Derivatives By Gas Chromatography-mass Spectrometry. J Chromatogr A. 2010 Oct 1;1217(40):6274-80. PubMed PMID: 20800845.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Analysis of phenylpiperazine-like stimulants in human hair as trimethylsilyl derivatives by gas chromatography-mass spectrometry. AU - Barroso,M, AU - Costa,S, AU - Dias,M, AU - Vieira,D N, AU - Queiroz,J A, AU - López-Rivadulla,M, Y1 - 2010/08/11/ PY - 2010/06/28/received PY - 2010/07/28/revised PY - 2010/08/02/accepted PY - 2010/8/31/entrez PY - 2010/8/31/pubmed PY - 2010/12/21/medline SP - 6274 EP - 80 JF - Journal of chromatography. A JO - J Chromatogr A VL - 1217 IS - 40 N2 - A simple and sensitive procedure, using p-tolylpiperazine (pTP) as internal standard (IS), has been developed and validated for the qualitative and quantitative analysis of 1-(3-trifuoromethylphenyl)piperazine (TFMPP), 1-(3-chlorophenyl)piperazine (mCPP) and 1-(4-methoxyphenyl)piperazine (MeOPP) in hair. Drug extraction was performed by incubation with 1 M sodium hydroxide at 50°C for 40 min, and the extracts were cleaned up using mixed-mode solid-phase extraction. The analytes were derivatized with N-methyl-N-(trimethylsilyl) trifluoroacetamide with 5% trimethylchlorosilane and analysed by gas chromatography-mass spectrometry in the selected ion monitoring mode. The method was linear from 0.05 (lower limit of quantitation) to 4 ng mg(-1), with correlation coefficients higher than 0.99 for all the compounds. Intra- and interday precision and accuracy were in conformity with the criteria normally accepted in bioanalytical method validation, and the sample cleanup step presented a mean efficiency higher than 90% for all the analytes. Due to its simplicity and speed, this method can be successfully applied in the screening and quantitation of these compounds in hair samples, and is suitable for application in forensic toxicology routine analysis. SN - 1873-3778 UR - https://www.unboundmedicine.com/medline/citation/20800845/Analysis_of_phenylpiperazine_like_stimulants_in_human_hair_as_trimethylsilyl_derivatives_by_gas_chromatography_mass_spectrometry_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0021-9673(10)01041-1 DB - PRIME DP - Unbound Medicine ER -