Broad-spectrum toxicological analysis of hair based on capillary zone electrophoresis-time-of-flight mass spectrometry

Rossella Gottardo, Ameriga Fanigliulo, Federica Bortolotti, Giorgia De Paoli, Jennifer Paola Pascali, Franco Tagliaro

    Research output: Contribution to journalArticle

    50 Citations (Scopus)

    Abstract

    The coupling of capillary electrophoresis-electrospray ionization and time-of-flight mass spectrometry, combining efficiency and speed of separation with high mass accuracy and fast scanning capability, was for the first time applied to the determination of drugs of abuse (amphetamine, methamphetamine, MDA, MDMA, ephedrine, cocaine, morphine, codeine) and their metabolites in hair (6-MAM, benzoylecgonine). Experimental conditions were as follows. Separation: voltage 15 kV, uncoated fused-silica capillary (75 p,m ID, 100 cm total length), running electrolyte 25 mM ammonium formate, pH 9.5, field-amplified sample stacking injection. Forensic drugs could be identified by exact mass determination (mass accuracy typically <= 5 ppm) and by match of the isotopic pattern. The method was fully validated, showing limit of detections (LODs) suitable for the determination of all the compounds below the cut-off usually adopted for hair analysis (0.1 ng/mg). Analytical precision in real matrices (tested at 0.1 and 1.0 ng/mg) was typically characterized by CV's <= 24% in both intra-day and day-to-day experiments. Quantitative determination was also tested by using a single internal standard (folcodine). Results, although with a moderate accuracy, conceivably depending on the lack of deuterated internal standards, proved useful for diagnostic use of the results from hair analysis. A single liquid-liquid extraction procedure was applied for all analytes, allowing the detection of a broad spectrum of basic drugs and their major metabolites. (c) 2007 Published by Elsevier B.V.

    Original languageEnglish
    Pages (from-to)190-197
    Number of pages8
    JournalJournal of Chromatography. A
    Volume1159
    Issue number1-2
    DOIs
    Publication statusPublished - 3 Aug 2007

    Fingerprint

    formic acid
    Capillary Electrophoresis
    Metabolites
    Electrophoresis
    Spectrum analysis
    Toxicology
    Mass spectrometry
    Mass Spectrometry
    Spectrum Analysis
    N-Methyl-3,4-methylenedioxyamphetamine
    Ephedrine
    Capillary electrophoresis
    Codeine
    Electrospray ionization
    Liquid-Liquid Extraction
    Methamphetamine
    Liquids
    Street Drugs
    Amphetamine
    Fused silica

    Cite this

    Gottardo, Rossella ; Fanigliulo, Ameriga ; Bortolotti, Federica ; De Paoli, Giorgia ; Pascali, Jennifer Paola ; Tagliaro, Franco. / Broad-spectrum toxicological analysis of hair based on capillary zone electrophoresis-time-of-flight mass spectrometry. In: Journal of Chromatography. A. 2007 ; Vol. 1159, No. 1-2. pp. 190-197.
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    title = "Broad-spectrum toxicological analysis of hair based on capillary zone electrophoresis-time-of-flight mass spectrometry",
    abstract = "The coupling of capillary electrophoresis-electrospray ionization and time-of-flight mass spectrometry, combining efficiency and speed of separation with high mass accuracy and fast scanning capability, was for the first time applied to the determination of drugs of abuse (amphetamine, methamphetamine, MDA, MDMA, ephedrine, cocaine, morphine, codeine) and their metabolites in hair (6-MAM, benzoylecgonine). Experimental conditions were as follows. Separation: voltage 15 kV, uncoated fused-silica capillary (75 p,m ID, 100 cm total length), running electrolyte 25 mM ammonium formate, pH 9.5, field-amplified sample stacking injection. Forensic drugs could be identified by exact mass determination (mass accuracy typically <= 5 ppm) and by match of the isotopic pattern. The method was fully validated, showing limit of detections (LODs) suitable for the determination of all the compounds below the cut-off usually adopted for hair analysis (0.1 ng/mg). Analytical precision in real matrices (tested at 0.1 and 1.0 ng/mg) was typically characterized by CV's <= 24{\%} in both intra-day and day-to-day experiments. Quantitative determination was also tested by using a single internal standard (folcodine). Results, although with a moderate accuracy, conceivably depending on the lack of deuterated internal standards, proved useful for diagnostic use of the results from hair analysis. A single liquid-liquid extraction procedure was applied for all analytes, allowing the detection of a broad spectrum of basic drugs and their major metabolites. (c) 2007 Published by Elsevier B.V.",
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    Gottardo, R, Fanigliulo, A, Bortolotti, F, De Paoli, G, Pascali, JP & Tagliaro, F 2007, 'Broad-spectrum toxicological analysis of hair based on capillary zone electrophoresis-time-of-flight mass spectrometry', Journal of Chromatography. A, vol. 1159, no. 1-2, pp. 190-197. https://doi.org/10.1016/j.chroma.2007.05.099

    Broad-spectrum toxicological analysis of hair based on capillary zone electrophoresis-time-of-flight mass spectrometry. / Gottardo, Rossella; Fanigliulo, Ameriga; Bortolotti, Federica; De Paoli, Giorgia; Pascali, Jennifer Paola; Tagliaro, Franco.

    In: Journal of Chromatography. A, Vol. 1159, No. 1-2, 03.08.2007, p. 190-197.

    Research output: Contribution to journalArticle

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    AU - Gottardo, Rossella

    AU - Fanigliulo, Ameriga

    AU - Bortolotti, Federica

    AU - De Paoli, Giorgia

    AU - Pascali, Jennifer Paola

    AU - Tagliaro, Franco

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    N2 - The coupling of capillary electrophoresis-electrospray ionization and time-of-flight mass spectrometry, combining efficiency and speed of separation with high mass accuracy and fast scanning capability, was for the first time applied to the determination of drugs of abuse (amphetamine, methamphetamine, MDA, MDMA, ephedrine, cocaine, morphine, codeine) and their metabolites in hair (6-MAM, benzoylecgonine). Experimental conditions were as follows. Separation: voltage 15 kV, uncoated fused-silica capillary (75 p,m ID, 100 cm total length), running electrolyte 25 mM ammonium formate, pH 9.5, field-amplified sample stacking injection. Forensic drugs could be identified by exact mass determination (mass accuracy typically <= 5 ppm) and by match of the isotopic pattern. The method was fully validated, showing limit of detections (LODs) suitable for the determination of all the compounds below the cut-off usually adopted for hair analysis (0.1 ng/mg). Analytical precision in real matrices (tested at 0.1 and 1.0 ng/mg) was typically characterized by CV's <= 24% in both intra-day and day-to-day experiments. Quantitative determination was also tested by using a single internal standard (folcodine). Results, although with a moderate accuracy, conceivably depending on the lack of deuterated internal standards, proved useful for diagnostic use of the results from hair analysis. A single liquid-liquid extraction procedure was applied for all analytes, allowing the detection of a broad spectrum of basic drugs and their major metabolites. (c) 2007 Published by Elsevier B.V.

    AB - The coupling of capillary electrophoresis-electrospray ionization and time-of-flight mass spectrometry, combining efficiency and speed of separation with high mass accuracy and fast scanning capability, was for the first time applied to the determination of drugs of abuse (amphetamine, methamphetamine, MDA, MDMA, ephedrine, cocaine, morphine, codeine) and their metabolites in hair (6-MAM, benzoylecgonine). Experimental conditions were as follows. Separation: voltage 15 kV, uncoated fused-silica capillary (75 p,m ID, 100 cm total length), running electrolyte 25 mM ammonium formate, pH 9.5, field-amplified sample stacking injection. Forensic drugs could be identified by exact mass determination (mass accuracy typically <= 5 ppm) and by match of the isotopic pattern. The method was fully validated, showing limit of detections (LODs) suitable for the determination of all the compounds below the cut-off usually adopted for hair analysis (0.1 ng/mg). Analytical precision in real matrices (tested at 0.1 and 1.0 ng/mg) was typically characterized by CV's <= 24% in both intra-day and day-to-day experiments. Quantitative determination was also tested by using a single internal standard (folcodine). Results, although with a moderate accuracy, conceivably depending on the lack of deuterated internal standards, proved useful for diagnostic use of the results from hair analysis. A single liquid-liquid extraction procedure was applied for all analytes, allowing the detection of a broad spectrum of basic drugs and their major metabolites. (c) 2007 Published by Elsevier B.V.

    U2 - 10.1016/j.chroma.2007.05.099

    DO - 10.1016/j.chroma.2007.05.099

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