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Rapid GC-MS confirmation of amphetamines in urine by extractive acylation.
Forensic Sci Int. 2009 Jan 10; 183(1-3):78-86.FS

Abstract

Amphetamine and related derivatives are widely abused central- and psychostimulants. Detection of certain derivatives, such as methcathinone, by commonly available immunoassay screening techniques is insufficient. Multi-analyte confirmations for amphetamine type stimulants are therefore required, but traditional gas chromatography-mass spectrometry methods necessitate lengthy analytical procedures with prolonged sample turn-around times. A validated rapid GC-MS assay for urinary confirmation of amphetamine, methamphetamine, methcathinone, ephedrine, norephedrine, methylenedioxyamphetamine, methylenedioxymethamphetamine, methylenedioxyethylamphetamine and N-methyl-1-(3,4 methylenedioxyphenyl)-2-butanamine is reported. The method entailed in situ derivatization of urine specimens by extractive acylation with pentafluoropropionic anhydride, followed by rapid chromatography on a microbore capillary column. Analytes were separated in less than 3 min and quantified simultaneously by selected-ion monitoring using stable isotope substituted internal standards. The total instrument cycle-time was 6 min per sample. The limits of detection were between 1.5 ng/mL and 6.25 ng/mL for the various analytes. Intermediate precision and accuracy were in the range of 6.3-13.8% and 90.5-107.3% for the respective analytes at the lower limit of quantitation, and between 5.8-12.6% and 95.4-103.1% for the high control. Long-term storage of methcathinone positive specimens at -20 degrees C proved insufficient stability of this analyte. The proposed assay is precise and accurate for confirmation of amphetamine and derivatives in urine. The complementary approach of extractive-derivatization and fast GC-MS analysis is especially applicable in routine clinical settings where reduced sample turn-around times are required. Further investigation of cathinone as a possible metabolite of methcathinone is warranted, based on results from analyzed authentic urine samples.

Authors+Show Affiliations

Department of Chemistry, University of Pretoria, Pretoria 0002, South Africa.No affiliation info available

Pub Type(s)

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

Language

eng

PubMed ID

19081690

Citation

Marais, Adriaan A S., and Johannes B. Laurens. "Rapid GC-MS Confirmation of Amphetamines in Urine By Extractive Acylation." Forensic Science International, vol. 183, no. 1-3, 2009, pp. 78-86.
Marais AA, Laurens JB. Rapid GC-MS confirmation of amphetamines in urine by extractive acylation. Forensic Sci Int. 2009;183(1-3):78-86.
Marais, A. A., & Laurens, J. B. (2009). Rapid GC-MS confirmation of amphetamines in urine by extractive acylation. Forensic Science International, 183(1-3), 78-86. https://doi.org/10.1016/j.forsciint.2008.10.021
Marais AA, Laurens JB. Rapid GC-MS Confirmation of Amphetamines in Urine By Extractive Acylation. Forensic Sci Int. 2009 Jan 10;183(1-3):78-86. PubMed PMID: 19081690.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Rapid GC-MS confirmation of amphetamines in urine by extractive acylation. AU - Marais,Adriaan A S, AU - Laurens,Johannes B, Y1 - 2008/12/10/ PY - 2008/09/26/received PY - 2008/10/28/revised PY - 2008/10/30/accepted PY - 2008/12/17/entrez PY - 2008/12/17/pubmed PY - 2009/5/20/medline SP - 78 EP - 86 JF - Forensic science international JO - Forensic Sci. Int. VL - 183 IS - 1-3 N2 - Amphetamine and related derivatives are widely abused central- and psychostimulants. Detection of certain derivatives, such as methcathinone, by commonly available immunoassay screening techniques is insufficient. Multi-analyte confirmations for amphetamine type stimulants are therefore required, but traditional gas chromatography-mass spectrometry methods necessitate lengthy analytical procedures with prolonged sample turn-around times. A validated rapid GC-MS assay for urinary confirmation of amphetamine, methamphetamine, methcathinone, ephedrine, norephedrine, methylenedioxyamphetamine, methylenedioxymethamphetamine, methylenedioxyethylamphetamine and N-methyl-1-(3,4 methylenedioxyphenyl)-2-butanamine is reported. The method entailed in situ derivatization of urine specimens by extractive acylation with pentafluoropropionic anhydride, followed by rapid chromatography on a microbore capillary column. Analytes were separated in less than 3 min and quantified simultaneously by selected-ion monitoring using stable isotope substituted internal standards. The total instrument cycle-time was 6 min per sample. The limits of detection were between 1.5 ng/mL and 6.25 ng/mL for the various analytes. Intermediate precision and accuracy were in the range of 6.3-13.8% and 90.5-107.3% for the respective analytes at the lower limit of quantitation, and between 5.8-12.6% and 95.4-103.1% for the high control. Long-term storage of methcathinone positive specimens at -20 degrees C proved insufficient stability of this analyte. The proposed assay is precise and accurate for confirmation of amphetamine and derivatives in urine. The complementary approach of extractive-derivatization and fast GC-MS analysis is especially applicable in routine clinical settings where reduced sample turn-around times are required. Further investigation of cathinone as a possible metabolite of methcathinone is warranted, based on results from analyzed authentic urine samples. SN - 1872-6283 UR - https://www.unboundmedicine.com/medline/citation/19081690/Rapid_GC_MS_confirmation_of_amphetamines_in_urine_by_extractive_acylation_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0379-0738(08)00426-X DB - PRIME DP - Unbound Medicine ER -