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Determination of methamphetamine enantiomer composition in human hair by non-chiral liquid chromatography-tandem mass spectrometry method.
J Chromatogr B Analyt Technol Biomed Life Sci. 2016 Aug 15; 1028:145-152.JC

Abstract

Chiral separation is crucial for investigating methamphetamine positive cases. While (S)-(+)-enantiomer of methamphetamine (S-MAMP) is a schedule II controlled substance, (R)-(-)-enantiomer (R-MAMP) is an active ingredient of a few over-the-counter drugs in the United States. Among biological specimen types, hair provides greater detection window than blood, urine or oral fluid, and are therefore regarded with particular interest. Herein we describe a novel non-chiral liquid chromatography-tandem mass spectrometry (LC-MS/MS) method to directly determine methamphetamine enantiomeric composition (percentage) in hair specimens. Hair samples were washed once with acetone, powdered, incubated overnight at 53°C in 0.1M hydrochloric acid (HCl), and subjected to a solid phase extraction (SPE). The extracts were derivatized using Marfey's reagent at 53°C for 60min. The final mixture was analyzed by LC-MS/MS. Chromatographic separation was achieved using a C18 Kinetex analytical column and 60% (v/v) aqueous methanol as mobile phase (isocratic). Triple quadrupole mass spectrometer was equipped with an electro-spray ionization (ESI) source operating in negative mode and the chromatograms were acquired using a multiple-reaction monitoring (MRM) approach. The results were expressed as ratio of R- to S-MAMP and then derived to composition percentages without requiring quantitating each enantiomer. The method was precise and accurate across 0-100% S-composition at a range of 80-18,000pg/mg. The performance of the new method was compared with an (S)-(-)-N-trifluoroacetylprolyl chloride (S-TPC) derivatization and gas chromatography-mass spectrometry (GC-MS) method on authentic methamphetamine-positive hair samples. Not only the new Marfey's reagent approach presented satisfactory correlation with the S-TPC approach, but it also exhibited significantly improved quality (e.g., S/N) of the chromatograms. In summary, our protocol employs cost effective and minimally hazardous Marfey's reagent to derivatize trace amounts of methamphetamine extracted from hair samples and a non-chiral LC-MS/MS approach to separate and identify the two enantiomers. The method allows determination of the methamphetamine enantiomeric composition without requiring quantitation of each enantiomer and is therefore well suited for further investigate previously determined methamphetamine positive cases. This method represents a viable tool for evaluation of long-term drug exposure.

Authors+Show Affiliations

United States Drug Testing Laboratories, Inc., 1700 S Mount Prospect Rd., Des Plaines, IL 60018, United States. Electronic address: irene.shu@usdtl.com.United States Drug Testing Laboratories, Inc., 1700 S Mount Prospect Rd., Des Plaines, IL 60018, United States.United States Drug Testing Laboratories, Inc., 1700 S Mount Prospect Rd., Des Plaines, IL 60018, United States.United States Drug Testing Laboratories, Inc., 1700 S Mount Prospect Rd., Des Plaines, IL 60018, United States.United States Drug Testing Laboratories, Inc., 1700 S Mount Prospect Rd., Des Plaines, IL 60018, United States.

Pub Type(s)

Journal Article
Validation Study

Language

eng

PubMed ID

27344045

Citation

Shu, Irene, et al. "Determination of Methamphetamine Enantiomer Composition in Human Hair By Non-chiral Liquid Chromatography-tandem Mass Spectrometry Method." Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, vol. 1028, 2016, pp. 145-152.
Shu I, Alexander A, Jones M, et al. Determination of methamphetamine enantiomer composition in human hair by non-chiral liquid chromatography-tandem mass spectrometry method. J Chromatogr B Analyt Technol Biomed Life Sci. 2016;1028:145-152.
Shu, I., Alexander, A., Jones, M., Jones, J., & Negrusz, A. (2016). Determination of methamphetamine enantiomer composition in human hair by non-chiral liquid chromatography-tandem mass spectrometry method. Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, 1028, 145-152. https://doi.org/10.1016/j.jchromb.2016.06.015
Shu I, et al. Determination of Methamphetamine Enantiomer Composition in Human Hair By Non-chiral Liquid Chromatography-tandem Mass Spectrometry Method. J Chromatogr B Analyt Technol Biomed Life Sci. 2016 Aug 15;1028:145-152. PubMed PMID: 27344045.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Determination of methamphetamine enantiomer composition in human hair by non-chiral liquid chromatography-tandem mass spectrometry method. AU - Shu,Irene, AU - Alexander,Amy, AU - Jones,Mary, AU - Jones,Joseph, AU - Negrusz,Adam, Y1 - 2016/06/11/ PY - 2015/12/03/received PY - 2016/06/08/revised PY - 2016/06/09/accepted PY - 2016/6/26/entrez PY - 2016/6/28/pubmed PY - 2017/2/18/medline KW - Enantiomer composition KW - Hair analysis KW - Marfey’s reagent KW - Non-chiral chromatography SP - 145 EP - 152 JF - Journal of chromatography. B, Analytical technologies in the biomedical and life sciences JO - J. Chromatogr. B Analyt. Technol. Biomed. Life Sci. VL - 1028 N2 - Chiral separation is crucial for investigating methamphetamine positive cases. While (S)-(+)-enantiomer of methamphetamine (S-MAMP) is a schedule II controlled substance, (R)-(-)-enantiomer (R-MAMP) is an active ingredient of a few over-the-counter drugs in the United States. Among biological specimen types, hair provides greater detection window than blood, urine or oral fluid, and are therefore regarded with particular interest. Herein we describe a novel non-chiral liquid chromatography-tandem mass spectrometry (LC-MS/MS) method to directly determine methamphetamine enantiomeric composition (percentage) in hair specimens. Hair samples were washed once with acetone, powdered, incubated overnight at 53°C in 0.1M hydrochloric acid (HCl), and subjected to a solid phase extraction (SPE). The extracts were derivatized using Marfey's reagent at 53°C for 60min. The final mixture was analyzed by LC-MS/MS. Chromatographic separation was achieved using a C18 Kinetex analytical column and 60% (v/v) aqueous methanol as mobile phase (isocratic). Triple quadrupole mass spectrometer was equipped with an electro-spray ionization (ESI) source operating in negative mode and the chromatograms were acquired using a multiple-reaction monitoring (MRM) approach. The results were expressed as ratio of R- to S-MAMP and then derived to composition percentages without requiring quantitating each enantiomer. The method was precise and accurate across 0-100% S-composition at a range of 80-18,000pg/mg. The performance of the new method was compared with an (S)-(-)-N-trifluoroacetylprolyl chloride (S-TPC) derivatization and gas chromatography-mass spectrometry (GC-MS) method on authentic methamphetamine-positive hair samples. Not only the new Marfey's reagent approach presented satisfactory correlation with the S-TPC approach, but it also exhibited significantly improved quality (e.g., S/N) of the chromatograms. In summary, our protocol employs cost effective and minimally hazardous Marfey's reagent to derivatize trace amounts of methamphetamine extracted from hair samples and a non-chiral LC-MS/MS approach to separate and identify the two enantiomers. The method allows determination of the methamphetamine enantiomeric composition without requiring quantitation of each enantiomer and is therefore well suited for further investigate previously determined methamphetamine positive cases. This method represents a viable tool for evaluation of long-term drug exposure. SN - 1873-376X UR - https://www.unboundmedicine.com/medline/citation/27344045/Determination_of_methamphetamine_enantiomer_composition_in_human_hair_by_non_chiral_liquid_chromatography_tandem_mass_spectrometry_method_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S1570-0232(16)30391-9 DB - PRIME DP - Unbound Medicine ER -