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Comparison of five derivatizing agents for the determination of amphetamine-type stimulants in human urine by extractive acylation and gas chromatography-mass spectrometry.
J Anal Toxicol. 2012 Jun; 36(5):340-4.JA

Abstract

Five acylation reagents have been compared for use as derivatizing agents for the analysis of amphetamine-type stimulants (ATS) in urine by gas chromatography-mass spectrometry (GC-MS). The evaluated reagents were heptafluorobutyric anhydride, pentafluoropropionic anhydride, trifluoroacetic anhydride, acetic anhydride (AA) and N-methyl-bis(trifluoroacetamide). The ATS included amphetamine, methamphetamine (MA), 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA) and 3,4-methylenedioxyethylamphetamine (MDEA). A mixture of the ATS was added to urine (1 mL) followed by KOH solution and saturated NaHCO(3) solution. The sample was then extracted with dichloromethane and the derivatizing agent and 2 µL were injected into the GC-MS instrument. The derivatizing agents were compared with reference to the signal-to-noise (S/N) ratios, peak area values, relative standard deviations (RSDs), linearities, limits of detection (LODs) and selectivities. The acetic anhydride proved to be the best according to the S/N ratio and peak area results for amphetamine, MA, MDMA and MDEA. The best RSD values of peak areas and of S/N ratios at 3 µg/mL were also given by AA in cases of MDA, MDMA and MDEA. At 20 µg/mL, the lowest RSD values of peak areas for MDA and the lowest RSD values of S/N ratios for MA, MDA, MDMA and MDEA were again given by AA. Additionally, the highest correlation coefficients for MA, MDA, MDMA and MDEA and the lowest LOD results for MA, MDMA and MDEA were produced by AA.

Authors+Show Affiliations

National Institute of Forensic Toxicology, H-1146 Budapest, Varannó utca 2-4, Hungary. dobosa@iszki.huNo affiliation info availableNo affiliation info available

Pub Type(s)

Comparative Study
Journal Article

Language

eng

PubMed ID

22582269

Citation

Dobos, Adrienn, et al. "Comparison of Five Derivatizing Agents for the Determination of Amphetamine-type Stimulants in Human Urine By Extractive Acylation and Gas Chromatography-mass Spectrometry." Journal of Analytical Toxicology, vol. 36, no. 5, 2012, pp. 340-4.
Dobos A, Hidvégi E, Somogyi GP. Comparison of five derivatizing agents for the determination of amphetamine-type stimulants in human urine by extractive acylation and gas chromatography-mass spectrometry. J Anal Toxicol. 2012;36(5):340-4.
Dobos, A., Hidvégi, E., & Somogyi, G. P. (2012). Comparison of five derivatizing agents for the determination of amphetamine-type stimulants in human urine by extractive acylation and gas chromatography-mass spectrometry. Journal of Analytical Toxicology, 36(5), 340-4. https://doi.org/10.1093/jat/bks026
Dobos A, Hidvégi E, Somogyi GP. Comparison of Five Derivatizing Agents for the Determination of Amphetamine-type Stimulants in Human Urine By Extractive Acylation and Gas Chromatography-mass Spectrometry. J Anal Toxicol. 2012;36(5):340-4. PubMed PMID: 22582269.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Comparison of five derivatizing agents for the determination of amphetamine-type stimulants in human urine by extractive acylation and gas chromatography-mass spectrometry. AU - Dobos,Adrienn, AU - Hidvégi,Elod, AU - Somogyi,Gábor Pál, PY - 2012/5/15/entrez PY - 2012/5/15/pubmed PY - 2012/9/11/medline SP - 340 EP - 4 JF - Journal of analytical toxicology JO - J Anal Toxicol VL - 36 IS - 5 N2 - Five acylation reagents have been compared for use as derivatizing agents for the analysis of amphetamine-type stimulants (ATS) in urine by gas chromatography-mass spectrometry (GC-MS). The evaluated reagents were heptafluorobutyric anhydride, pentafluoropropionic anhydride, trifluoroacetic anhydride, acetic anhydride (AA) and N-methyl-bis(trifluoroacetamide). The ATS included amphetamine, methamphetamine (MA), 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA) and 3,4-methylenedioxyethylamphetamine (MDEA). A mixture of the ATS was added to urine (1 mL) followed by KOH solution and saturated NaHCO(3) solution. The sample was then extracted with dichloromethane and the derivatizing agent and 2 µL were injected into the GC-MS instrument. The derivatizing agents were compared with reference to the signal-to-noise (S/N) ratios, peak area values, relative standard deviations (RSDs), linearities, limits of detection (LODs) and selectivities. The acetic anhydride proved to be the best according to the S/N ratio and peak area results for amphetamine, MA, MDMA and MDEA. The best RSD values of peak areas and of S/N ratios at 3 µg/mL were also given by AA in cases of MDA, MDMA and MDEA. At 20 µg/mL, the lowest RSD values of peak areas for MDA and the lowest RSD values of S/N ratios for MA, MDA, MDMA and MDEA were again given by AA. Additionally, the highest correlation coefficients for MA, MDA, MDMA and MDEA and the lowest LOD results for MA, MDMA and MDEA were produced by AA. SN - 1945-2403 UR - https://www.unboundmedicine.com/medline/citation/22582269/Comparison_of_five_derivatizing_agents_for_the_determination_of_amphetamine_type_stimulants_in_human_urine_by_extractive_acylation_and_gas_chromatography_mass_spectrometry_ L2 - https://academic.oup.com/jat/article-lookup/doi/10.1093/jat/bks026 DB - PRIME DP - Unbound Medicine ER -