Gas Chromatography Multiresidue Method for Enantiomeric Fraction Determination of Psychoactive Substances in Effluents and River Surface Waters
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Determination of psychoactive substances (PAS) and/or their metabolites in surface waters is crucial for environmental risk assessment, and disclosure of their enantiomeric fractions (EF) allows discrimination between consumption, direct disposal, and synthesis pathways. The aim of this study was to develop and validate an indirect method by gas chromatography coupled to mass spectrometry (GC–MS) based on derivatization using (R)-(−)-α-methoxy-α-(trifluoromethyl) phenylacetyl chloride as chiral derivatization reagent, for enantiomeric quantification of amphetamine (AMP), methamphetamine (MAMP), 3,4-methylenedioxymethamphetamine (MDMA), norketamine, buphedrone (BPD), butylone, 3,4-dimethylmethcathinone (3,4-DMMC), 3-methylmethcathinone, and quantification of 1-benzylpiperazine and 1-(4-metoxyphenyl)-piperazine. The method allowed to evaluate the occurrence, spatial distribution, and the EF of the target chiral PAS in Portuguese surface waters and in effluents from 2 wastewater treatment plants (WWTP). For that, water samples were pre-concentrated by solid phase extraction using OASIS® MCX cartridges, derivatized and further analyzed by GC–MS. Both enantiomers of AMP, (R)-MDMA, (S)-MAMP, and the first eluted enantiomer of BPD (configuration not assigned) were found in surface waters, while effluent samples showed both enantiomers of MDMA, (S)-MAMP, (R)-AMP, and the first eluted enantiomer of BPD and 3,4-DMMC. According to our knowledge, this is the first multiresidue analytical method by CG–MS enrolling cathinones, amphetamines, and piperazines. The presence of illicit synthetic cathinones in Douro River estuary is here reported for the first time, along with other amphetamine derivatives. The potential of the method to monitor consumption of the target PAS was demonstrated.Keywords:
Designer drug
Solid phase extraction
Solid phase extraction
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BSTFA
Trimethylsilyl
Dimethyl formamide
Tetrahydrofuran
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Trimethylsilyl
BSTFA
Sonication
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BSTFA
Trimethylsilyl
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A method for analyzing belladonna alkaloids--hyoscyamine, scopolamine, anisodamine and anisodine, by means of capillary GC and GC-MSD was described. The retention data and characteristic ions of the parent and TMS derivatives of these alkaloids are given and will be very useful for identification of unknown alkaloids. The derivatization of different silylation reagents was compared, and the derivatization with MSTFA was found to be better than with BSA and BSTFA. The method has been used for studying biotransformation of these alkaloids in biosynthesis. Analysis of anisodamine and anisodine by CGC and GC-MS has not been found in the literature. In addition, the advantages of TMS derivatization are also discussed.
Anisodamine
BSTFA
Hyoscyamine
Scopolamine
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Designer drug
Drugs of abuse
Forensic Toxicology
Solid phase extraction
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A new and rapid microwave assisted derivatization method for the determination of fatty acids in edible oil by GC MS was developed. The optimum conditions for derivatization, such as the derivatization solvent composition, microwave assisted derivatization pressure and time were studied for KOH methanol and H 2SO 4 methanol systems. The experimental results were compared with those obtained by traditional method of normal temperature derivatization .The applied range of the two derivatization systems was also discussed in detail. The derivatization was accomplished in 1 minute. Heptane was used as extraction solvent. The method is rapid, efficient, accurate and solvent saving.
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Abstract Studies are described on the metabolism and toxicological analysis of the piperazine‐derived designer drug 1‐(3,4‐methylenedioxybenzyl)piperazine (MDBP) in rat urine using gas chromatography/mass spectrometry (GC/MS). The identified metabolites indicated that MDBP was metabolized by demethylenation and subsequent methylation to N ‐(4‐hydroxy‐3‐methoxybenzyl)piperazine followed by partial glucuronidation or sulfation. Additionally, degradation of the piperazine moiety to N ‐(3,4‐methylenedioxybenzyl)ethylenediamine and 3,4‐methylenedioxybenzylamine and N ‐dealkylation to piperazine were observed. The authors' systematic toxicological analysis (STA) procedure using full‐scan GC/MS after acid hydrolysis, liquid/liquid extraction and microwave‐assisted acetylation allowed the detection of MDBP and its above‐mentioned metabolites in rat urine after single administration of a dose calculated from the doses commonly taken by drug users. Assuming similar metabolism, the described STA procedure should be suitable for proof of an intake of MDBP by analysis of human urine. Copyright © 2004 John Wiley & Sons, Ltd.
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Piperazine
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The effects of different deproteinization and derivatization methods in serum sample preparation on metabolome were compared by gas chromatography-mass spectrometry.The relative standard derivations(RSD) of peak area and information content of profile were calculated.The principal components analysis(PCA),qualitative and quantitative analysis of serum samples and quality control samples(QC) were done.The RSD of QC and serum samples was less than 10%.The result of information content and PCA showed that these serum preparation methods were stable and reliable.The PCA result of profile produced by four preparation methods showed that the differences existed in serum metabolome when the samples were deproteinized and derivatizated by different reagents in preparation procedures.The influence of derivatization reagents on serum metabolome was great than that of deproteinization reagents.The information content of samples derivatizated by N-methyl-N-(trimethylsilyl) trifluoroacetamide(MSTFA)(8.9) was higher than that of samples derivatizated by BSTFA(8.7).Forty-four metabolites were obtained by qualitative analysis.Five metabolites were unique to samples derivatizated by MSTFA,and six metabolites were unique to samples derivatizated by N,O-Bis(trimethylsilyl) trifluoroacetamide(BSTFA).We proposed that when polar amino acids and short-chain fatty acids were concerned,BSTFA was recommended as derivatization reagent,and when nonpolar amino acids and long-chain fatty acids were concerned,MSTFA was recommended as derivatization reagent.
BSTFA
Metabolome
Trimethylsilyl
Sample Preparation
Quantitative Analysis
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The study of the biotransformation of a new synthetic drug 2,5-dimethoxy-4-bromamphetamine (DOB) and identification of its metabolites in urine of a poisoned person is described using gas chromatography mass spectrometry (GC-MS) with various ways of derivatization. It has been confirmed that one of its metabolic pathways leads to the corresponding 2-O-desmethyl and 5-O-desmethyl metabolites when the latter is prevailing. It is important to know the metabolism of this neurotoxic and hallucinogenic substance as it is a prerequisite for developing reliable toxicological diagnostic procedures and for assessment of toxicological risks.
Biotransformation
Designer drug
Desmethyl
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