Determination of cocaine, its metabolites, pyrolysis products, and ethanol adducts in postmortem fluids and tissues using Zymark® automated solid-phase extraction and gas chromatography-mass spectrometry1

Lewis, Russell J.; Johnson, Robert D.; Angier, M.K; Ritter, Roxane M.

doi:10.1016/j.jchromb.2004.03.045

Cited by 28 publications

(11 citation statements)

References 45 publications

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“…In GC analysis, it is known that BE and NCOC need a derivatization step to improve its volatility due to the presence of a polar functional group in its molecular structure [28,29]. As the temperature of incubation for the chosen silylating agent, MSTFA, varies from author to author [30][31][32][33][34], the effectiveness of this derivatization procedure was evaluated using 3 different temperatures: 37, 55, and 80 • C. The main objective was to verify if cocaine chemical stability would be affected by the derivatization temperature.…”

Section: Choice Of Suitable Derivatization Temperaturementioning

confidence: 99%

Development and validation of a gas chromatography/ion trap-mass spectrometry method for simultaneous quantification of cocaine and its metabolites benzoylecgonine and norcocaine: Application to the study of cocaine metabolism in human primary cultured renal cells

Valente¹,

Carvalho²,

Bastos³

et al. 2010

Journal of Chromatography B

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Section: Choice Of Suitable Derivatization Temperaturementioning

confidence: 99%

Development and validation of a gas chromatography/ion trap-mass spectrometry method for simultaneous quantification of cocaine and its metabolites benzoylecgonine and norcocaine: Application to the study of cocaine metabolism in human primary cultured renal cells

Valente¹,

Carvalho²,

Bastos³

et al. 2010

Journal of Chromatography B

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“…Surprisingly, normorphine, an analyte rarely monitored, was detected in the next highest number of specimens (42). If free morphine was employed to identify opiate exposure, many positive specimens would be missed as only 12 of 119 contained this analyte.…”

Section: Resultsmentioning

confidence: 99%

“…Although neither is psychoactive, these biomarkers are highly effective in detecting cocaine exposure because of their long half-lives in urine. According to Lewis and coworkers, BE concentration in urine was 2–3-fold higher than EME in five postmortem cases analyzed for cocaine and metabolites by GC–MS (42). Cardona et al (43) also confirmed the presence of BE in higher concentrations than EME.…”

Section: Discussionmentioning

confidence: 99%

Simultaneous Liquid Chromatography-Mass Spectrometry Quantification of Urinary Opiates, Cocaine, and Metabolites in Opiate-Dependent Pregnant Women in Methadone-Maintenance Treatment

Shakleya

Dams²,

Choo

et al. 2010

Journal of Analytical Toxicology

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Opiates, cocaine, and metabolites were quantified by liquid chromatography–mass spectrometry (LC–MS) in 284 urine specimens, collected thrice weekly, to monitor possible drug relapse in 15 pregnant heroin-dependent women. Opiates were detected in 149 urine specimens (52%) with limits of quantification (LOQ) of 10–50 μg/L. Morphine, morphine-3-glucuronide, and/or morphine-6-glucuronide were positive in 121 specimens; 6-acetylmorphine, a biomarker of heroin ingestion, was quantifiable in only 7. No heroin, 6-acetylcodeine, papaverine, or noscapine were detected. One hundred and sixty-five urine specimens (58%) from all 15 participants were positive for one or more cocaine analytes (LOQ 10–100 μg/L). Ecgonine methylester (EME) and/or benzoylecgonine were the major cocaine biomarkers in 142. Anhydroecgonine methylester, a biomarker of smoked cocaine, was positive in six; cocaethylene and/or ecgonine ethylester, biomarkers of cocaine and ethanol co-ingestion, were found in 25. At the current Substance Abuse Mental Health Services Administration cutoffs for total morphine (2000 μg/L), codeine (2000 μg/L), 6-acetylmorphine (10 μg/L), and benzoylecgonine (100 μg/L), 16 opiate- and 29 cocaine-positive specimens were identified. Considering 100 μg/L EME as an additional urinary cocaine biomarker would identify 51 more positive cocaine specimens. Of interest is the differential pattern of opiate and cocaine biomarkers observed after LC–MS as compared to gas chromatography–mass spectrometry analysis.

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“…Outros trabalhos utilizando a pirólise analítica ou os produtos de pirólise para identificar a presença de drogas e seus metabólicos no sangue, na urina ou em tecidos humanos têm sido feitos [114][115][116][117][118] . Neste sentido, Mitsui et al 119 aplicaram a pirólise para estudar narcóticos e sais de alcalóides em urinas de seres humanos.…”

Section: Ciência Forenseunclassified

A pirólise como técnica analítica

Silvério¹,

Barbosa²,

Piló‐Veloso³

2008

Quím. Nova

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Recebido em 16/4/07; aceito em 31/10/07; publicado na web em 7/8/08PYROLYSIS AS AN ANALYTICAL TECHNIQUE. In this paper historical aspects of analytical pyrolysis, the equipment used, the fundamentals and the mechanisms of pyrolysis of different polymeric materials are discussed. The latest work on analytical pyrolysis applied to various types of synthetic and natural samples is reviewed. Current applications of this technique that are discussed include identification of microorganisms, analysis of trace compounds by forensic laboratories, investigation of food and agricultural products, study of the chemical composition of wood, authentication and conservation of artworks, and the study of environmental and geochemical samples.Keywords: Py-GC-MS; degradation mechanism; polymeric materials. introDUÇÃoA palavra pirólise possui origem grega e significa "decomposição pelo calor", ou seja, a degradação de um material por energia tér-mica. No entanto, pirólise analítica é uma técnica de caracterização de determinado material, na ausência de oxigênio, pelas reações de degradação químicas induzidas por energia térmica.1 Esse processo resulta em um conjunto de pequenas espécies moleculares, as quais são relacionadas à composição da amostra original. 1,2Essas pequenas moléculas são usadas para identificar qualitativamente a estrutura original de macromoléculas, por meio de padronização própria e adequada, e para fornecer informação quantitativa da sua composição. 3A pirólise qualitativa caracteriza-se por ser uma técnica em que constantemente se realizam comparações de pirogramas de referência (impressões digitais) com pirolisados de interesse. 4 Nesse tipo de análise, a reprodutibilidade dos resultados é obtida quando os parâ-metros que levam à formação desses pirolisados são minuciosamente controlados e otimizados para um sistema polimérico investigado, pois esses influenciam diretamente nos mecanismos de degradação térmica.5 Em amostras poliméricas, os mecanismos dessas fragmentações podem ocorrer via eliminação de pequenas moléculas, cisão de cadeia (despolimerização) ou clivagem aleatória. 6 Como a degradação térmica de macromoléculas freqüentemente produz misturas complexas de moléculas menores, é necessário o uso associado de outras técnicas, como a cromatografia em fase gasosa, para promover a separação das espécies produzidas.7 Quando essa associação ou acoplamento inclui também a espectrometria de massas, as espécies produzidas podem ser ainda identificadas (Figura 1).Se a degradação resultar em reações secundárias indesejáveis resultando em sinais mais alargados, 8 ou se ocorrer perdas de produtos de degradação durante a transferência do pirolisador para o sistema cromatográfico, 9 a alternativa mais indicada é o acoplamento do pirolisador diretamente ao espectrômetro de massas, originando a técnica de análise conhecida pela sigla Pi-EM. 10Esta revisão foi motivada pela escassa literatura em português sobre esse tema. Assim, este artigo objetiva apresentar os fundamentos da pirólise como técnica analítica e inv...

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Determination of cocaine, its metabolites, pyrolysis products, and ethanol adducts in postmortem fluids and tissues using Zymark® automated solid-phase extraction and gas chromatography-mass spectrometry1

Cited by 28 publications

References 45 publications

Development and validation of a gas chromatography/ion trap-mass spectrometry method for simultaneous quantification of cocaine and its metabolites benzoylecgonine and norcocaine: Application to the study of cocaine metabolism in human primary cultured renal cells

Development and validation of a gas chromatography/ion trap-mass spectrometry method for simultaneous quantification of cocaine and its metabolites benzoylecgonine and norcocaine: Application to the study of cocaine metabolism in human primary cultured renal cells

Simultaneous Liquid Chromatography-Mass Spectrometry Quantification of Urinary Opiates, Cocaine, and Metabolites in Opiate-Dependent Pregnant Women in Methadone-Maintenance Treatment

A pirólise como técnica analítica

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