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Novel Method for the Determination of Urinary Phenylamine Abused Drugs Using Gas Chromatography-Mass Spectrometry
Dissertation

Novel Method for the Determination of Urinary Phenylamine Abused Drugs Using Gas Chromatography-Mass Spectrometry

Min-Kun Huang
Doctor of Philosophy (PHD), 國立清華大學, 化學系
2005

Abstract

氣相層析質譜儀 尿液 安非他命類 愷他命 固相微萃取 GC-MS Urine Amphetamines Ketamine SPME
Abstract In this thesis, we have completed four articles focused on the detection of some abused phenalkylamines found in Taiwan and the other countries. Solid-phase microextraction (SPME) and solid-phase extraction (SPE) methods were applied to extract these drugs and some of their metabolites in urine, then these compounds were derivatized with Heptafluorobutyric anhydride/Heptafluorobutyric chloride (HFBA/HFBCl) or MBTFA to yield more volatile, more stable, higher molecular weight, and easily detectable targets for GC-MS using selected ion monitoring mode (SIM). In the first article, we extracted amphetamine (AMP) and methamphetamine (MTH) using headspace-SPME method, and finished the derivatization procedure on the SPME fiber at the same time. After gas chromatography-mass spectrometry (GC-MS) injection, we got about 10 % of recovery for both of AMP and MTH. In the second article, we applied a high boiling point acylation reagent, N-methyl-bis(trifluoroacetamide) (CF3CONCH3COCF3, MBTFA), to derivatize and detect ketamine (KT), norketamine (NK), and dehydronorketamine (DHNK). This proposed process achieves high sensitivity to detect these three compounds. The analytical method was also applied to determine the concentration of KT, NK, and DHNK in some suspected urine specimens. Because polydrug abuse were found in recent years, an analytical method for simultaneous determination of MTH, AMP, 3,4-methylenedioxymethamphetamine (MDMA), 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxyethylamphetamine (MDEA), KT, NK, and DHNK in urine is described in the third article. The sample preparation and detection method is similar as those in the second article. Excellent linear regression, overall recoveries, and detection limit is obtained for all of these eight compounds. In the last article, an analytical method for simultaneous determination of some new abused drugs, 4-bromo-2,5-dimethoxyphenethylamine (2C-B), 4-chloro-2,5-dimethoxyphenethylamine (2C-C), and 4-iodo-2,5-dimethoxyphenethylamine (2C-I), is developed. Because the lack of these halogenated compound in the commercial market, the standards should be synthesized in the laboratory. The analysis of these drugs is based on SPE and chemical derivatization (ChD) using MBTFA. These derivatized compounds are then separated and detected using GC-MS. Like the other three developed methods, excellent method validation results were achieved. Although we have completed four studies, but more advanced studies in this related field may be proceeded continuously, such as using MBTFA to replace HFBA/HBCl as ChD reagent in the one step SPME procedure, extracting and derivatizing KT in the SPME method, or detectinging AMP, KT and 2C-Bs simultaneously in the SPE process.

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