Single-step procedure for gas chromatography–mass spectrometry screening and quantitative determination of amphetamine-type stimulants and related drugs in blood, serum, oral fluid and urine samples

Kankaanpää, Aino; Gunnar, Teemu; Ariniemi, Kari; Lillsunde, Pirjo; Mykkänen, Sirpa; Seppαlä, Timo

doi:10.1016/j.jchromb.2004.07.035

Cited by 49 publications

(24 citation statements)

References 43 publications

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“…Alcoholic functional groups such as the b-hydroxy groups of NE, NPE, EPH and PEP remained underivatized after the initial acylation reaction. No mixed derivatives of mono-(mono-N-PFP) and diacylated (bis-N,O-PFP) compounds in appreciable yield were found as reported in the extractive-derivatization technique of Kankaanpä ä et al [21]. Formation of the diacylated derivatives of NE, NPE, EPH and PEP was preferred, as better chromatographic resolution and separation speed was achieved.…”

Section: Discussionmentioning

confidence: 81%

“…A total instrumental cycle-time of 6 min per sample was obtained, which compares favourably with current rapid chromatographic methodologies for both GC-MS and LC-MS/MS [16,21]. The total sample preparation time for a batch of 20 specimens, performed by a single analyst, was approximately 45 min.…”

Section: Gc-ms Analysismentioning

confidence: 76%

“…Analytical strategies including gas chromatography (GC) [12,13], high performance liquid chromatography (HPLC) [14,15], gas chromatography-mass spectrometry (GC-MS) [10,12,[16][17][18][19][20][21] and liquid chromatography-tandem mass spectrometry (LC-MS/MS) [22,23] have been employed. The majority of samples received by our laboratory are direct confirmation requests by clinicians.…”

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confidence: 99%

“…Recent work that has focused on such multianalyte procedures has shown their applicability in a routine laboratory setting [21][22][23]. LC-MS/MS procedures [22,23] have the advantage of decreased work-up time due to the ability to analyse underivatized compounds.…”

mentioning

confidence: 99%

“…Currently, GC-MS is still the preferred method for forensic confirmation in urine [25] and has the advantage of lower equipment costs. Utilizing a single step extractive-derivatization technique with heptafluorobutyric anhydride (HFBA), it has been shown that derivatization need not be a timely step in GC-MS sample preparation procedures for amphetamines [21]. Aside from direct injection methodologies that may suffer from their own pitfalls such as ion suppression/ enhancement, similar sample preparation times for GC-MS and LC-MS/MS thus exist.…”

mentioning

confidence: 99%

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Rapid GC–MS confirmation of amphetamines in urine by extractive acylation

Marais

Laurens

2009

Forensic Science International

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Section: Discussionmentioning

confidence: 81%

Section: Gc-ms Analysismentioning

confidence: 76%

mentioning

confidence: 99%

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confidence: 99%

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confidence: 99%

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Rapid GC–MS confirmation of amphetamines in urine by extractive acylation

Marais

Laurens

2009

Forensic Science International

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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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Differentiation of ring‐substituted regioisomers of cathinone analogs by supercritical fluid chromatography

Segawa

Kusakabe

Ishii

et al. 2020

Analytical Science Advances

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Various new psychoactive substances, such as cathinone and its analogs, possess similar chemical structures. Accurate identification of structurally similar drugs of abuse is important in forensic drug analysis. Chromatographic differentiation is a powerful analytical technique for this purpose. In this study, we applied supercritical fluid chromatography to differentiate ring-substituted regioisomers of six synthetic cathinone analogs (fluoro-𝛼-pyrrolidinovalerophenone, methyl-𝛼-pyrrolidinovalerophenone, methoxy-𝛼pyrrolidinovalerophenone, fluoro-𝛼-pyrrolidinooctanophenone, fluoropentedrone, and fluorooctedrone). The examined cathinone analogs were weakly retained on the stationary phase (possessing diol functional group) and eluted quickly. We optimized the conditions to retain the examined cathinone analogs to achieve sufficient separation, and found that the types of functional groups on the stationary phase greatly affected the retention and separation. Systematic examination of the chromatographic conditions showed that the two stationary phases possessing anthracene and pentafluorobenzyl groups had good separation capabilities for the examined 2-, 3-, and 4regioisomers of six cathinone analogs, which had different skeletal structures. Interestingly, the two stationary phases showed different selectivities, and alteration of the elution order was observed. The developed method was validated and its discrimination ability was investigated by measuring mass spectra and absorption spectra. Supercritical fluid chromatography-ultraviolet absorption spectroscopy/mass spectrometry is a powerful analytical technique for differentiation of ring-substituted cathinone analogs.

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Single-step procedure for gas chromatography–mass spectrometry screening and quantitative determination of amphetamine-type stimulants and related drugs in blood, serum, oral fluid and urine samples

Cited by 49 publications

References 43 publications

Rapid GC–MS confirmation of amphetamines in urine by extractive acylation

Rapid GC–MS confirmation of amphetamines in urine by extractive acylation

Chemical Reagents and Derivatization Procedures in Drug Analysis

Differentiation of ring‐substituted regioisomers of cathinone analogs by supercritical fluid chromatography

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