title: Chemometrics-assisted chromatographic fingerprinting: An illicit methamphetamine case study.
abstract: The volatile chemical constituents in complex mixtures can be analyzed using gas chromatography with mass spectrometry. This analysis allows the tentative identification of diverse impurities of an illicit methamphetamine sample. The acquired two-dimensional data of liquid-liquid extraction was resolved by multivariate curve resolution alternating curve resolution to elucidate the embedded peaks effectively. This is the first report on the application of a curve resolution approach for chromatogram fingerprinting to identify particularly the embedded impurities of a drug of abuse. Indeed, the strong and broad peak of methamphetamine makes identifying the underlying peaks problematic and even impossible. Mathematical separation instead of conventional chromatographic approaches was performed in a way that trace components embedded in methamphetamine peak were successfully resolved. Comprehensive analysis of the chromatogram, using multivariate curve resolution, resulted in elution profiles and mass spectra for each pure compound. Impurities such as benzaldehyde, benzyl alcohol, benzene, propenyl methyl ketone, benzyl methyl ketone, amphetamine, N-benzyl-2-methylaziridine, phenethylamine, N,N,α-trimethylamine, phenethylamine, N,α,α-trimethylmethamphetamine, N-acetylmethamphetamine, N-formylmethamphetamine, and other chemicals were identified. A route-specific impurity, N-benzyl-2-methylaziridine, indicating a synthesis route based on ephedrine/pseudoephedrine was identified. Moreover, this is the first report on the detection of impurities such as phenethylamine, N,α,α-trimethylamine (a structurally related impurity), and clonitazene (as an adulterant) in an illicit methamphetamine sample.
authors.affiliation: Department of Clean Technologies, Chemistry and Chemical Engineering Research Center of Iran, Tehran, Iran.
authors.forename: Nafiseh
authors.initials: N
authors.lastname: Shekari
authors.affiliation: Department of Clean Technologies, Chemistry and Chemical Engineering Research Center of Iran, Tehran, Iran.
authors.forename: Maryam
authors.initials: M
authors.lastname: Vosough
authors.affiliation: Department of Clean Technologies, Chemistry and Chemical Engineering Research Center of Iran, Tehran, Iran.
authors.forename: Kourosh
authors.initials: K
authors.lastname: Tabar Heidar
mesh_terms: D004340:Drug Contamination; D008401:Gas Chromatography-Mass Spectrometry; D013287:Illicit Drugs / Q000032:analysis*; D008694:Methamphetamine / Q000032:analysis*
chemical_list: D013287:Illicit Drugs; D008694:Methamphetamine
keywords: curve resolution; embedded peaks; fingerprinting; illicit methamphetamine; impurity profiling