GC–MS determination of amphetamines in serum using on-line trifluoroacetylation

Hidvégi, Előd; Fabian, P.; Hideg, Z. S.; Somogyi, G.

doi:10.1016/j.forsciint.2006.03.030

Cited by 23 publications

(13 citation statements)

References 13 publications

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“…For such purpose, analytical data are obtained to identify 2,5-DMA and related analogues by measuring their proton nuclear magnetic resonance ( 1 H NMR) spectra, infrared (IR) spectra, and mass spectra [1]. In addition, analysis of these hallucinogens by thinlayer chromatography (TLC) [1], gas chromatography-mass spectrometry (GC-MS) [1,7,[8][9][10], gas chromatography/tandem mass spectrometry (GC/MS/MS) [7] and liquid chromatographymass spectrometry (LC-MS) [1] has been reported. The determination of amphetamines has been also performed using HPLC-UV [11], capillary electrophoresis (CE) with diode array detection [12] and the on-line combination of CE and MS which has been established as a powerful method in forensic screening analysis [2].…”

Section: Introductionmentioning

confidence: 99%

GC–MS and GC–IRD studies on dimethoxyamphetamines (DMA): Regioisomers related to 2,5-DMA

Maher

Awad

DeRuiter

et al. 2009

Forensic Science International

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Section: Introductionmentioning

confidence: 99%

GC–MS and GC–IRD studies on dimethoxyamphetamines (DMA): Regioisomers related to 2,5-DMA

Maher

Awad

DeRuiter

et al. 2009

Forensic Science International

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“…The sample preparation for several samples Forensic Toxicol could be completed in less than 10 min, including 5 min for centrifugation. It was much quicker than the methods using LLE [10,20] or SPE [26,27] with evaporation, especially with low evaporation temperature. In this study, the addition of acid was not needed, and no extra timeconsuming derivatization steps were involved, which proved to be much simpler than many other methods [20,23,28].…”

Section: Development Of the Pretreatment Proceduresmentioning

confidence: 96%

“…Some researchers have prevented the evaporation of amphetamines by adding acid [9,20], using a low evaporation temperature [18,21], or trapping analytes by means of derivatization before the highly volatile eluate is evaporated to dryness [22]. Even after derivatization, the compounds needed to be evaporated under low temperatures in order to avoid the evaporation of AMP and MAMP [23].…”

Section: Introductionmentioning

confidence: 99%

Simple and rapid analysis of four amphetamines in human whole blood and urine using liquid–liquid extraction without evaporation/derivatization and gas chromatography–mass spectrometry

et al. 2014

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We developed a simple and rapid analysis method for the determination of four amphetamines in human whole blood and urine using gas chromatographymass spectrometry (GC-MS). During the course of sample preparation, the evaporation process was found to be the weak point for amphetamine and methamphetamine analysis. Liquid-liquid extraction in this study was conducted without the evaporation step, and the upper solvent layer was injected directly without derivatization, which effectively prevented the volatile amphetamines from vanishing during evaporation and guaranteed the linearity of the calibration curves. This method showed good selectivity, precision, and accuracy, and at the same time was simple and fast. The limits of detection were 5 ng/ml. As an application of this study, a whole blood sample and urine sample from a drug abuse suspect were analyzed. This method may be able to meet the need for rapid and accurate confirmation of positive immunoassay results as well as quantification in clinical and forensic toxicological cases. To our knowledge, no forensic toxicologists have noted that such a basic and simple method, without evaporation or derivatization, is useful for routine analysis of amphetamines using GC-MS.

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“…(22) On-line flash injection of extracted amphetamines with MBTFA provided GC/MS separation and identification of 12 compounds at limits of detection of 2.5-6.9 ng mL −1 . (23) Perfluoro acid anhydrides [R (C=O)-O(C=O)R ], such as trifluoro-, pentafluoro-, and heptafluoro-acid anhydride (TFAA, trifluoroacetic anhydride; PFAA, pentafluoropropionic anhydride; HFAA, heptafluorobutyric anhydride) react readily with alcohols, phenols, and urine for the preparation of perfluoroacyl derivatives, which are particularly useful for EC detection ( Table 2, reagent 2). Triethylamine is added, as part of the reaction mixture, to neutralize the acidic by-products and drive the reaction to completion.…”

Section: Acylationmentioning

confidence: 99%

Chemical Reagents and Derivatization Procedures in Drug Analysis

Danielson

Gallagher

Bao

2008

Encyclopedia of Analytical Chemistry

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This article describes both pre‐ and postcolumn derivatization chemistry used in conjunction with either chromatography or capillary electrophoresis (CE) to facilitate the determination of drugs. Generally, only prederivatization is used in gas chromatography (GC), principally to enhance the volatility, temperature stability, and/or detectability. The GC section considers derivatization of drugs by reagent class: alkylation, acylation, and silylation. The GC sample‐handling section describes an approach that combines the extraction and derivatization steps together. Both pre‐ and postcolumn derivatization are common approaches for high‐performance liquid chromatography (HPLC) and many of these methods have been adapted for CE. Derivatization for HPLC is often directed toward aliphatic amines, carboxylic acids, or alcohols that are difficult to detect at low levels by absorbance, luminescence, or electrochemical means. In addition, small hydrophilic molecules upon prederivatization are often converted into larger more hydrophobic compounds, making reversed‐phase HPLC easier or even feasible. The HPLC section considers derivatization of drugs based on the following types: alkaloids, amines, antibiotics, barbiturates, carbonyl compounds and carboxylic acids, catecholamines, hydroxy compounds, steroids, and sulfur compounds. For the GC and HPLC sections, tables are included, giving the structures of the more important derivatizing agents, the analytes, and the corresponding reaction products. A brief rationale for derivatization chemistry with CE concludes this article. For CE, derivatization is often done to improve detectability as the path length for absorbance detection is very short and fluorescence can be effective using laser‐based systems.

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GC–MS determination of amphetamines in serum using on-line trifluoroacetylation

Cited by 23 publications

References 13 publications

GC–MS and GC–IRD studies on dimethoxyamphetamines (DMA): Regioisomers related to 2,5-DMA

GC–MS and GC–IRD studies on dimethoxyamphetamines (DMA): Regioisomers related to 2,5-DMA

Simple and rapid analysis of four amphetamines in human whole blood and urine using liquid–liquid extraction without evaporation/derivatization and gas chromatography–mass spectrometry

Chemical Reagents and Derivatization Procedures in Drug Analysis

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