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Negative ion chemical ionization for the determination of methylphenidate in human plasma by stable isotope dilution gas chromatography/mass spectrometry.
J Mass Spectrom. 2000 Sep; 35(9):1100-4.JM

Abstract

A sensitive and specific method for the determination of methylphenidate in human plasma is presented. Methylphenidate was extracted from plasma by solvent extraction with hexane at pH 9.3 and derivatized to its heptafluorobutyrate derivative. The derivative was measured by gas chromatography/negative ion chemical ionization mass spectrometry without any further purification. Using this detection mode, a diagnostically useful fragment ion at m/z 369 was obtained at high relative abundance. (18)O(2)-labelled methylphenidate was used as an internal standard and its rapid and facile preparation from the unlabeled compound is described. Calibration graphs were linear within the range 0.14-18.25 ng ml(-1). The inter-assay precision was 8.7% (0.14 ng ml(-1)) and 3.1% (4.56 ng ml(-1)) and the intra-assay variability was 1.3% (0.14 ng ml(-1)) and 0.4% (4.56 ng ml(-1)). Accuracy determinations showed deviations of +0.7% (0.14 ng ml(-1)) and -2.5% (4.56 ng ml(-1)). The method is rugged, rapid and robust and has been applied to the batch analysis of methylphenidate during pharmacokinetic profiling of the drug.

Authors+Show Affiliations

University Children's Hospital, Department of Analytical Biochemistry and Mass Spectrometry, Auenbruggerplatz 30, A-8036 Graz, Austria. hans.leis@kfunigraz.ac.atNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

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

Language

eng

PubMed ID

11006603

Citation

Leis, H J., et al. "Negative Ion Chemical Ionization for the Determination of Methylphenidate in Human Plasma By Stable Isotope Dilution Gas Chromatography/mass Spectrometry." Journal of Mass Spectrometry : JMS, vol. 35, no. 9, 2000, pp. 1100-4.
Leis HJ, Fauler G, Raspotnig G, et al. Negative ion chemical ionization for the determination of methylphenidate in human plasma by stable isotope dilution gas chromatography/mass spectrometry. J Mass Spectrom. 2000;35(9):1100-4.
Leis, H. J., Fauler, G., Raspotnig, G., & Windischhofer, W. (2000). Negative ion chemical ionization for the determination of methylphenidate in human plasma by stable isotope dilution gas chromatography/mass spectrometry. Journal of Mass Spectrometry : JMS, 35(9), 1100-4.
Leis HJ, et al. Negative Ion Chemical Ionization for the Determination of Methylphenidate in Human Plasma By Stable Isotope Dilution Gas Chromatography/mass Spectrometry. J Mass Spectrom. 2000;35(9):1100-4. PubMed PMID: 11006603.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Negative ion chemical ionization for the determination of methylphenidate in human plasma by stable isotope dilution gas chromatography/mass spectrometry. AU - Leis,H J, AU - Fauler,G, AU - Raspotnig,G, AU - Windischhofer,W, PY - 2000/9/28/pubmed PY - 2001/2/28/medline PY - 2000/9/28/entrez SP - 1100 EP - 4 JF - Journal of mass spectrometry : JMS JO - J Mass Spectrom VL - 35 IS - 9 N2 - A sensitive and specific method for the determination of methylphenidate in human plasma is presented. Methylphenidate was extracted from plasma by solvent extraction with hexane at pH 9.3 and derivatized to its heptafluorobutyrate derivative. The derivative was measured by gas chromatography/negative ion chemical ionization mass spectrometry without any further purification. Using this detection mode, a diagnostically useful fragment ion at m/z 369 was obtained at high relative abundance. (18)O(2)-labelled methylphenidate was used as an internal standard and its rapid and facile preparation from the unlabeled compound is described. Calibration graphs were linear within the range 0.14-18.25 ng ml(-1). The inter-assay precision was 8.7% (0.14 ng ml(-1)) and 3.1% (4.56 ng ml(-1)) and the intra-assay variability was 1.3% (0.14 ng ml(-1)) and 0.4% (4.56 ng ml(-1)). Accuracy determinations showed deviations of +0.7% (0.14 ng ml(-1)) and -2.5% (4.56 ng ml(-1)). The method is rugged, rapid and robust and has been applied to the batch analysis of methylphenidate during pharmacokinetic profiling of the drug. SN - 1076-5174 UR - https://www.unboundmedicine.com/medline/citation/11006603/Negative_ion_chemical_ionization_for_the_determination_of_methylphenidate_in_human_plasma_by_stable_isotope_dilution_gas_chromatography/mass_spectrometry_ L2 - https://doi.org/10.1002/1096-9888(200009)35:9<1100::AID-JMS32>3.0.CO;2-9 DB - PRIME DP - Unbound Medicine ER -