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Simultaneous determination of amphetamine and methamphetamine enantiomers in urine by simultaneous liquid-liquid extraction and diastereomeric derivatization followed by gas chromatographic-isotope dilution mass spectrometry.
J Chromatogr B Analyt Technol Biomed Life Sci. 2005 Feb 25; 816(1-2):131-43.JC

Abstract

A simple, rapid, reliable, and economic analytical scheme starting with in situ liquid-liquid extraction and asymmetric (or diastereomeric) chemical derivatization (ChD) followed by gas chromatography (GC)-isotope dilution mass spectrometry (MS) is described for the simultaneous determination of D- and L-amphetamine (AP) and methamphetamine (MA) in urine which could have resulted from the administration of various forms of questioned amphetamines or amphetamines-generating drugs. By using L-N-trifluoroacetyl-1-prolyl chloride (L-TPC) as chiral derivatizing agent, resolutions of 2.2 and 2.0 were achieved for the separation of AP and MA enantiomeric pairs, respectively, on an ordinary HP-5MS capillary column. The GC-MS quantitation was carried out in the selected ion monitoring (SIM) mode using m/z 237 and 251 as the quantifier ions for the respective diastereomeric pairs of AP-L-TPC and MA-L-TPC. The calibration curves plotted for the two pairs of analytes stretch with good linearity down to 45 ng/mL, and the limits of detection and quantitation determined were as low as 40 and 45 ng/mL, respectively. Also, a comparative study using 10 real-case urine specimens previously screened as positive for MA administration showed mostly tolerable biases between the two sums (of concentration) of D- and L-MA obtained via an asymmetric L-TPC-ChD approach and via an ordinary pentafluoropropionylation (PFPA-ChD) approach, respectively, as well as between the two sums of D- and L-AP obtained thereupon, thus validating the proposed analytical scheme as a promising forensic protocol for the detailed analysis of enantiomeric amphetamines in urine.

Authors+Show Affiliations

Department of Forensic Science, Central Police University, Kueishan, Taoyuan 33334, Taiwan, ROC. wang531088@sun4.cpu.edu.twNo affiliation info availableNo affiliation info available

Pub Type(s)

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

Language

eng

PubMed ID

15664343

Citation

Wang, Sheng-Meng, et al. "Simultaneous Determination of Amphetamine and Methamphetamine Enantiomers in Urine By Simultaneous Liquid-liquid Extraction and Diastereomeric Derivatization Followed By Gas Chromatographic-isotope Dilution Mass Spectrometry." Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, vol. 816, no. 1-2, 2005, pp. 131-43.
Wang SM, Wang TC, Giang YS. Simultaneous determination of amphetamine and methamphetamine enantiomers in urine by simultaneous liquid-liquid extraction and diastereomeric derivatization followed by gas chromatographic-isotope dilution mass spectrometry. J Chromatogr B Analyt Technol Biomed Life Sci. 2005;816(1-2):131-43.
Wang, S. M., Wang, T. C., & Giang, Y. S. (2005). Simultaneous determination of amphetamine and methamphetamine enantiomers in urine by simultaneous liquid-liquid extraction and diastereomeric derivatization followed by gas chromatographic-isotope dilution mass spectrometry. Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, 816(1-2), 131-43.
Wang SM, Wang TC, Giang YS. Simultaneous Determination of Amphetamine and Methamphetamine Enantiomers in Urine By Simultaneous Liquid-liquid Extraction and Diastereomeric Derivatization Followed By Gas Chromatographic-isotope Dilution Mass Spectrometry. J Chromatogr B Analyt Technol Biomed Life Sci. 2005 Feb 25;816(1-2):131-43. PubMed PMID: 15664343.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Simultaneous determination of amphetamine and methamphetamine enantiomers in urine by simultaneous liquid-liquid extraction and diastereomeric derivatization followed by gas chromatographic-isotope dilution mass spectrometry. AU - Wang,Sheng-Meng, AU - Wang,Ting-Cheng, AU - Giang,Yun-Seng, PY - 2003/11/05/received PY - 2004/11/10/accepted PY - 2005/1/25/pubmed PY - 2005/6/1/medline PY - 2005/1/25/entrez SP - 131 EP - 43 JF - Journal of chromatography. B, Analytical technologies in the biomedical and life sciences JO - J. Chromatogr. B Analyt. Technol. Biomed. Life Sci. VL - 816 IS - 1-2 N2 - A simple, rapid, reliable, and economic analytical scheme starting with in situ liquid-liquid extraction and asymmetric (or diastereomeric) chemical derivatization (ChD) followed by gas chromatography (GC)-isotope dilution mass spectrometry (MS) is described for the simultaneous determination of D- and L-amphetamine (AP) and methamphetamine (MA) in urine which could have resulted from the administration of various forms of questioned amphetamines or amphetamines-generating drugs. By using L-N-trifluoroacetyl-1-prolyl chloride (L-TPC) as chiral derivatizing agent, resolutions of 2.2 and 2.0 were achieved for the separation of AP and MA enantiomeric pairs, respectively, on an ordinary HP-5MS capillary column. The GC-MS quantitation was carried out in the selected ion monitoring (SIM) mode using m/z 237 and 251 as the quantifier ions for the respective diastereomeric pairs of AP-L-TPC and MA-L-TPC. The calibration curves plotted for the two pairs of analytes stretch with good linearity down to 45 ng/mL, and the limits of detection and quantitation determined were as low as 40 and 45 ng/mL, respectively. Also, a comparative study using 10 real-case urine specimens previously screened as positive for MA administration showed mostly tolerable biases between the two sums (of concentration) of D- and L-MA obtained via an asymmetric L-TPC-ChD approach and via an ordinary pentafluoropropionylation (PFPA-ChD) approach, respectively, as well as between the two sums of D- and L-AP obtained thereupon, thus validating the proposed analytical scheme as a promising forensic protocol for the detailed analysis of enantiomeric amphetamines in urine. SN - 1570-0232 UR - https://www.unboundmedicine.com/medline/citation/15664343/Simultaneous_determination_of_amphetamine_and_methamphetamine_enantiomers_in_urine_by_simultaneous_liquid_liquid_extraction_and_diastereomeric_derivatization_followed_by_gas_chromatographic_isotope_dilution_mass_spectrometry_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S1570-0232(04)00942-0 DB - PRIME DP - Unbound Medicine ER -