Identification of sympathomimetic alkylamine agents in urine using liquid chromatography–mass spectrometry and comparison of derivatization methods for confirmation analyses by gas chromatography–mass spectrometry

Sardela, Vinícius Figueiredo; Sardela, P.D.O.; Deventer, Koen; Araujo, Amanda Lessa Dutra de; Cavalcante, Karina M.; Padilha, Marina; Pereira, Henrique Marcelo Gualberto; Eenoo, Peter Van; Neto, Francisco Radler de Aquino

doi:10.1016/j.chroma.2013.05.016

Cited by 14 publications

(6 citation statements)

References 29 publications

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“…25,26 First, with the addition of MSTFA, the silylation of the amine and hydroxy groups occurred, as already observed in the previous derivatization. When added, MBTFA reacted with the molecules by replacing the trimethylsilyl group attached to the nitrogen with a trifluoroacetyl group through a nucleophilic substitution reaction of the SN 2 type.…”

Section: Mstfa/mbtfa Evaluationmentioning

confidence: 75%

Fast Ephedrine Quantification by Gas Chromatography Mass Spectrometry

Carneiro¹,

Silva²,

Cavalcante³

et al. 2018

J. Braz. Chem. Soc.

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Ephedrines are widely used in therapy. Because of their stimulant properties, these substances are relevant in different forensic fields. At present, the state of the art for ephedrines quantification relay based on a liquid chromatography mass spectrometry, mainly because of the dilute-andshoot approach. Notwithstanding, several gas chromatography based methods have already been described, all of them include cleanup steps, with the potential disadvantage of incurring errors and increasing the workload. In this paper, a straightforward method for ephedrine quantification based on gas chromatographic mass spectrometry, without cleanup and based on Doehlert matrix optimization is presented. Only 10 µL of a urine sample is necessary and for N-methyl-N-(trimethylsilyl)trifluoroacetamide/N-methyl-bis-trifluoracetamide derivatives, the intermediate precision was 2.77% for ephedrine, 9.20% for cathine, 8.29% for norephedrine and 4.27% for pseudoephedrine. The limit of detection was 20 ng mL -1 for ephedrine, 30 ng mL -1 for cathine and 40 ng mL -1 for norephedrine and pseudoephedrine.

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Section: Mstfa/mbtfa Evaluationmentioning

confidence: 75%

Fast Ephedrine Quantification by Gas Chromatography Mass Spectrometry

Carneiro¹,

Silva²,

Cavalcante³

et al. 2018

J. Braz. Chem. Soc.

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“…The analytical method was adapted from the earlier publication by Thevis et al . The analyses were performed using the same GC‐MS system described by Sardela et al …”

Section: Methodsmentioning

confidence: 99%

“…By the same token, confirmation of suspicious (presumptive analytical findings) samples must apply a mass spectrometric method. [12] To the best of our knowledge, qualitative/quantitative detection methods for glycerol in the field of doping analysis are limited to the Thevis et al [7] publication. This method was established using a gas chromatography-isotope dilution mass spectrometry-based approach under linearity between 1.0 to 98.0 μgmL À1 with an overnight step to dry the urine for the subsequent derivatization.…”

Section: Introductionmentioning

confidence: 99%

“…Screening of glycerol can be similarly performed by a colourimetric method. By the same token, confirmation of suspicious (presumptive analytical findings) samples must apply a mass spectrometric method . To the best of our knowledge, qualitative/quantitative detection methods for glycerol in the field of doping analysis are limited to the Thevis et al .…”

Section: Introductionmentioning

confidence: 99%

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Systematic analysis of glycerol: colourimetric screening and gas chromatography–mass spectrometric confirmation

Sardela

Scalco

Cavalcante

et al. 2015

Drug Testing and Analysis

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Glycerol is a naturally occurring polyol in the human body, essential for several metabolic processes. It is widely used in the food, pharmaceutical, and medical industries and in clinical practice as a plasma volume expander (PVE). Athletes, however, may use glycerol to mask the presence of forbidden substances or to enhance performance, inclusively through hyperhydration achieved by glycerol ingestion with added fluid. These practices are considered doping, and are prohibited by the World Anti-Doping Agency (WADA). Therefore, glycerol was introduced in the prohibited list. Doping through glycerol ingestion can readily be identified by detection of elevated glycerol concentrations in urine. In this paper, a protocol for the fast detection of glycerol in urine is proposed. It consists of a previous visual colourimetric screening, followed by a quantitative/qualitative confirmation analysis by mass spectrometry. The screening procedure involves a reaction in which polyhydric alcohols are oxidized by periodate to formic acid and formaldehyde, which is detected by the addition of a fuchsin solution. For the subsequent qualitative/quantitative confirmation analysis, a gas chromatography-mass spectrometry based approach with a non-deuterated internal standard and a drying step of only 10 min is proposed. The linear correlation was demonstrated within WADA´s threshold range. The calculated RSD were 2.1% for within-day precision and 2.8% for between-day precision. The uncertainty estimation was calculated, and a value of 2.7% was obtained. The procedure may also be used for the analysis of other polyols in urine, as for example the PVE mannitol.

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“…For the stereospecificity investigation, the sample preparation was performed as described by Sardela et al 19 Briefly, a liquid-liquid extraction (LLE) was conducted with a 2 mL aliquot from each tank using 5 mL of hexane after the addition of phentermine (I.S., final concentration at 1 μg/mL). Then, 60 μL of Mosher:hexane solution 2% (v/ v) and 120 μL of aqueous 5 M potassium hydroxide were added.…”

Section: For Stereospecificity Investigationmentioning

confidence: 99%

Zebrafish (Danio rerio) water tank model for the investigation of drug metabolism: Progress, outlook, and challenges

Sardela

Anselmo

Nunes

et al. 2018

Drug Testing and Analysis

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Zebrafish (Danio rerio) water tank (ZWT) approach was investigated as an alternative model for metabolism studies based on six different experiments with four model compounds. Sibutramine was applied for the multivariate optimization of ZWT conditions, also for the comparison of the metabolism among ZWT, humans and mice, beyond for the role of CYP2B6 in ZWT. After the optimization, 18 fish and 168 hours of experiments is the minimum requirement for a relevant panel of biotransformation products. A comparison among the species resulted in the observation of the same hydroxylated metabolites, with differences in metabolites concentration ratio. However, the ZWT allowed tuning of the conditions to obtain a specific metabolic profile, depending on the need. In addition, by utilizing CYP2B6 inhibition, a relevant ZWT pathway for the demethylation of drugs was determined. The stereospecificity of the ZWT metabolism was investigated using selegiline and no racemization or inversion transformations were observed. Moreover, the investigation of metabolism of cannabimimetics was performed using JWH-073 and the metabolites observed are the same described for humans, except for the hydroxylation at the indol group, which was explained by the absence of CYP2C9 orthologs in zebrafish. Finally, hexarelin was used as a model to evaluate studies by ZWT for drugs with low stability.As a result, hexarelin displays a very fast metabolization in ZWT conditions and all the metabolites described for human were observed in ZWT. Therefore, the appropriate conditions, merits, and relevant limitations to conduct ZWT experiments for the investigation of drug metabolism are described.

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Identification of sympathomimetic alkylamine agents in urine using liquid chromatography–mass spectrometry and comparison of derivatization methods for confirmation analyses by gas chromatography–mass spectrometry

Cited by 14 publications

References 29 publications

Fast Ephedrine Quantification by Gas Chromatography Mass Spectrometry

Fast Ephedrine Quantification by Gas Chromatography Mass Spectrometry

Systematic analysis of glycerol: colourimetric screening and gas chromatography–mass spectrometric confirmation

Zebrafish (Danio rerio) water tank model for the investigation of drug metabolism: Progress, outlook, and challenges

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