Development of Analytical Methods for the Detection of Metaraminol in the Horse*

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Published: Journal of Analytical Toxicology, ISSN 0146-4760, Volume 24, Number 4, May/June 2000, pp. 275-280

Chemical Derivatization and the Selection of Deuterated Internal Standard for Quantitative Determination—Methamphetamine Example* Use of an isotopic analogue of the analyte as the internal standard in a quantitative gas chromatography–mass spectrometry targeted-compound-analysis protocol is often hindered by the availability of an adequate number (typically three for the drug/metabolite and two for the isotopic analogue) of sufficiently high mass ions that can be attributed to each member of the pair and are sufficiently free of interference by the contribution from the other component of the pair, a phenomenon termed “cross-contribution”. Methamphetamine (MA) is selected as the exemplar compound to examine the effectiveness in using different chemical derivatization routes to produce derivatized analyte-isotopic analogue pairs that can generate more favorable mass spectrometric data to meet this analytical requirement. Trimethylsilyl-, trichloroacetyl-, and pentafluoropropionyl-derivatization and MA-d5, MA-d8, and MA-d9 are studied. Data resulting from this study indicate that the number of ion pairs suitable for quantitation and the degree of cross-contribution of these ions vary significantly. These data empirically demonstrate that derivatization methods play a significant role in deciding which deuterated analogue of the analyte provides the most suitable ion pairs that cause the least cross-contribution. The most suitable internal standard varies with the derivatization route adapted for an analytical protocol.Dong-Liang Lin
Ministry of Justice Bureau of Investigation, Taipei, Taiwan
Wei-Tun Chang
Department of Forensic Science, Central Police University, Taoyuan, Taiwan
Tsung-Li Kuo
Department of Legal Medicine, College of Medicine, National Taiwan University, Taipei, Taiwan
Ray H. Liu
Graduate Program in Forensic Science, University of Alabama at Birmingham, Birmingham, Alabama 35294

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