Analysis of phenylpiperazine-like stimulants in human hair as trimethylsilyl derivatives by gas chromatography-mass spectrometry.
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.
Barroso
M
M
Instituto Nacional de Medicina Legal-Delegação do Sul, Rua Manuel Bento de Sousa, 3, 1150-219 Lisboa, Portugal. mbarroso@dlinml.mj.pt
Costa
S
S
Dias
M
M
Vieira
D N
DN
Queiroz
J A
JA
López-Rivadulla
M
M
D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006197:Hair / Q000737:chemistry*; D006801:Humans; D016018:Least-Squares Analysis; D010879:Piperazines / Q000032:analysis* / Q000737:chemistry; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D014297:Trimethylsilyl Compounds / Q000032:analysis* / Q000737:chemistry
D010879:Piperazines; D014297:Trimethylsilyl Compounds; C039293:trimethylchlorosilane; C031503:phenylpiperazine