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Simultaneous determination of eight sympathomimetic amines in urine by gas chromatography/mass spectrometry.
J AOAC Int. 2010 Jan-Feb; 93(1):116-22.JA

Abstract

A GC method was developed for the identification and quantitation of eight sympathomimetic amines in urine, i.e., amphetamine, methamphetamine, mephentermine, ephedrine, pseudoephedrine, methylenedioxyamphetamine, methylenedioxymethamphetamine, and methylenedioxyethylamphetamine. Methoxyphenamine was used as the internal standard (IS). The assay is rapid, sensitive, and simple to perform. It involves a liquid-liquid extraction procedure with simultaneous in-solution derivatization of the organic layer with pentafluorobenzoyl chloride (PFB-CI), followed by GC/MS analysis. These derivatives and the IS were extracted from 1 mL alkaline urine into hexane before derivatization with PFB-CI. The organic layer was then removed and evaporated to dryness before dissolution with hexane for GC/MS analysis. Calibration curves for each analyte showed linearity in the range of 25-5000 ng/mL (r2 > or = 0.997). Recoveries ranged from 88 to 99%, with the precision of recoveries typically < or = 5%. The LOD values ranged from 7 to 28 ng/mL, and the LOQ values ranged from 23 to 94 ng/mL. At least four ions were available for each analyte for confirmation of identity by MS.

Authors+Show Affiliations

University of Western Sydney, College of Health and Science, Centre for Complementary Medicine Research, Herbal Analysis and Pharmacological Laboratory, P.O. Box 1797, Penrith South DC, 1797, NSW, Australia.No affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

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

Language

eng

PubMed ID

20334173

Citation

Moawad, Michael, et al. "Simultaneous Determination of Eight Sympathomimetic Amines in Urine By Gas Chromatography/mass Spectrometry." Journal of AOAC International, vol. 93, no. 1, 2010, pp. 116-22.
Moawad M, Khoo CS, Lee S, et al. Simultaneous determination of eight sympathomimetic amines in urine by gas chromatography/mass spectrometry. J AOAC Int. 2010;93(1):116-22.
Moawad, M., Khoo, C. S., Lee, S., & Hennell, J. R. (2010). Simultaneous determination of eight sympathomimetic amines in urine by gas chromatography/mass spectrometry. Journal of AOAC International, 93(1), 116-22.
Moawad M, et al. Simultaneous Determination of Eight Sympathomimetic Amines in Urine By Gas Chromatography/mass Spectrometry. J AOAC Int. 2010 Jan-Feb;93(1):116-22. PubMed PMID: 20334173.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Simultaneous determination of eight sympathomimetic amines in urine by gas chromatography/mass spectrometry. AU - Moawad,Michael, AU - Khoo,Cheang S, AU - Lee,Samiuela, AU - Hennell,James R, PY - 2010/3/26/entrez PY - 2010/3/26/pubmed PY - 2010/5/4/medline SP - 116 EP - 22 JF - Journal of AOAC International JO - J AOAC Int VL - 93 IS - 1 N2 - A GC method was developed for the identification and quantitation of eight sympathomimetic amines in urine, i.e., amphetamine, methamphetamine, mephentermine, ephedrine, pseudoephedrine, methylenedioxyamphetamine, methylenedioxymethamphetamine, and methylenedioxyethylamphetamine. Methoxyphenamine was used as the internal standard (IS). The assay is rapid, sensitive, and simple to perform. It involves a liquid-liquid extraction procedure with simultaneous in-solution derivatization of the organic layer with pentafluorobenzoyl chloride (PFB-CI), followed by GC/MS analysis. These derivatives and the IS were extracted from 1 mL alkaline urine into hexane before derivatization with PFB-CI. The organic layer was then removed and evaporated to dryness before dissolution with hexane for GC/MS analysis. Calibration curves for each analyte showed linearity in the range of 25-5000 ng/mL (r2 > or = 0.997). Recoveries ranged from 88 to 99%, with the precision of recoveries typically < or = 5%. The LOD values ranged from 7 to 28 ng/mL, and the LOQ values ranged from 23 to 94 ng/mL. At least four ions were available for each analyte for confirmation of identity by MS. SN - 1060-3271 UR - https://www.unboundmedicine.com/medline/citation/20334173/Simultaneous_determination_of_eight_sympathomimetic_amines_in_urine_by_gas_chromatography/mass_spectrometry_ DB - PRIME DP - Unbound Medicine ER -