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Accelerated quantification of amphetamine enantiomers in human urine using chiral liquid chromatography and on-line column-switching coupled with tandem mass spectrometry.
Anal Bioanal Chem. 2017 Feb; 409(5):1291-1300.AB

Abstract

Amphetamine (AM) is a powerful psychostimulant existing in two enantiomeric forms. Stereoselective analysis of AM in biosamples can assist clinicians and forensic experts in differentiating between abuse of illicitly synthesized racemic AM and ingestion of pharmaceutical AM formulations containing either S-AM or different proportions of the S- and R-enantiomers. Therefore, a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for quantifying AM enantiomers in urine was newly developed. The method comprised dilution with water, followed by injection of the diluted sample onto an achiral C18 trapping column for purification and subsequent backflush elution to a chiral Lux 3 μm AMP LC column by means of a switching valve. An isocratic mobile phase of 25 % acetonitrile in 0.1 M aqueous ammonia was used for enantiomeric separation. Injection, cleanup, and backflush of the next sample were performed before the previous sample had eluted from the analytical column, thus enabling simultaneous enantioseparation of up to three samples within the analytical column. This novel chromatographic concept allowed for increased sample throughput by accelerating both the sample preparation and the LC analysis. Analyte detection was accomplished by electrospray ionization in positive ion mode and selected reaction monitoring using a triple-stage quadrupole mass spectrometer. The method was successfully validated through assessment of its linearity, lower limit of quantification, accuracy and precision, selectivity, matrix effect, carry-over, dilution integrity, and re-injection reproducibility. Linearity ranged from 0.05 to 25 mg/L for both enantiomers. Proof of the method included analysis of urine samples obtained from drug abusers and patients receiving an S-AM prodrug. Graphical Abstract Enantioselective determination of amphetamine in human urine using liquid chromatography with achiral-chiral column-switching and tandem mass spectrometry.

Authors+Show Affiliations

Institute of Forensic Medicine, University of Bern, Bühlstrasse 20, 3012, Bern, Switzerland.Institute of Forensic Medicine, University of Bern, Bühlstrasse 20, 3012, Bern, Switzerland.Institute of Forensic Medicine, University of Bern, Bühlstrasse 20, 3012, Bern, Switzerland.Phenomenex, Zeppelinstrasse 5, 63741, Aschaffenburg, Germany.Institute of Forensic Medicine, University of Bern, Bühlstrasse 20, 3012, Bern, Switzerland. stefan.koenig@irm.unibe.ch.

Pub Type(s)

Journal Article
Validation Study

Language

eng

PubMed ID

27838752

Citation

Hädener, Marianne, et al. "Accelerated Quantification of Amphetamine Enantiomers in Human Urine Using Chiral Liquid Chromatography and On-line Column-switching Coupled With Tandem Mass Spectrometry." Analytical and Bioanalytical Chemistry, vol. 409, no. 5, 2017, pp. 1291-1300.
Hädener M, Bruni PS, Weinmann W, et al. Accelerated quantification of amphetamine enantiomers in human urine using chiral liquid chromatography and on-line column-switching coupled with tandem mass spectrometry. Anal Bioanal Chem. 2017;409(5):1291-1300.
Hädener, M., Bruni, P. S., Weinmann, W., Frübis, M., & König, S. (2017). Accelerated quantification of amphetamine enantiomers in human urine using chiral liquid chromatography and on-line column-switching coupled with tandem mass spectrometry. Analytical and Bioanalytical Chemistry, 409(5), 1291-1300. https://doi.org/10.1007/s00216-016-0056-1
Hädener M, et al. Accelerated Quantification of Amphetamine Enantiomers in Human Urine Using Chiral Liquid Chromatography and On-line Column-switching Coupled With Tandem Mass Spectrometry. Anal Bioanal Chem. 2017;409(5):1291-1300. PubMed PMID: 27838752.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Accelerated quantification of amphetamine enantiomers in human urine using chiral liquid chromatography and on-line column-switching coupled with tandem mass spectrometry. AU - Hädener,Marianne, AU - Bruni,Pia S, AU - Weinmann,Wolfgang, AU - Frübis,Matthias, AU - König,Stefan, Y1 - 2016/11/12/ PY - 2016/08/12/received PY - 2016/10/24/accepted PY - 2016/09/22/revised PY - 2016/11/14/pubmed PY - 2018/3/10/medline PY - 2016/11/14/entrez KW - Chiral separation KW - Column-switching chromatography KW - LC-MS/MS KW - R-/S-amphetamine KW - Urine SP - 1291 EP - 1300 JF - Analytical and bioanalytical chemistry JO - Anal Bioanal Chem VL - 409 IS - 5 N2 - Amphetamine (AM) is a powerful psychostimulant existing in two enantiomeric forms. Stereoselective analysis of AM in biosamples can assist clinicians and forensic experts in differentiating between abuse of illicitly synthesized racemic AM and ingestion of pharmaceutical AM formulations containing either S-AM or different proportions of the S- and R-enantiomers. Therefore, a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for quantifying AM enantiomers in urine was newly developed. The method comprised dilution with water, followed by injection of the diluted sample onto an achiral C18 trapping column for purification and subsequent backflush elution to a chiral Lux 3 μm AMP LC column by means of a switching valve. An isocratic mobile phase of 25 % acetonitrile in 0.1 M aqueous ammonia was used for enantiomeric separation. Injection, cleanup, and backflush of the next sample were performed before the previous sample had eluted from the analytical column, thus enabling simultaneous enantioseparation of up to three samples within the analytical column. This novel chromatographic concept allowed for increased sample throughput by accelerating both the sample preparation and the LC analysis. Analyte detection was accomplished by electrospray ionization in positive ion mode and selected reaction monitoring using a triple-stage quadrupole mass spectrometer. The method was successfully validated through assessment of its linearity, lower limit of quantification, accuracy and precision, selectivity, matrix effect, carry-over, dilution integrity, and re-injection reproducibility. Linearity ranged from 0.05 to 25 mg/L for both enantiomers. Proof of the method included analysis of urine samples obtained from drug abusers and patients receiving an S-AM prodrug. Graphical Abstract Enantioselective determination of amphetamine in human urine using liquid chromatography with achiral-chiral column-switching and tandem mass spectrometry. SN - 1618-2650 UR - https://www.unboundmedicine.com/medline/citation/27838752/Accelerated_quantification_of_amphetamine_enantiomers_in_human_urine_using_chiral_liquid_chromatography_and_on_line_column_switching_coupled_with_tandem_mass_spectrometry_ L2 - https://dx.doi.org/10.1007/s00216-016-0056-1 DB - PRIME DP - Unbound Medicine ER -