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1.
Int J Legal Med ; 130(2): 393-400, 2016 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-26671597

RESUMO

Phosphatidylethanol (PEth) is considered as specific biomarker of alcohol consumption. Due to accumulation after repeated drinking, PEth is suitable to monitor long-term drinking behavior. To examine the applicability of PEth in "driving under the influence of alcohol" cases, 142 blood samples with blood alcohol concentrations (BAC) ranging from 0.0-3.12‰ were analyzed for the presence of PEth homologues 16:0/18:1 (889 ± 878 ng/mL; range

Assuntos
Alcoolismo/sangue , Dirigir sob a Influência , Glicerofosfolipídeos/sangue , Adolescente , Adulto , Idoso , Idoso de 80 Anos ou mais , Biomarcadores/sangue , Cromatografia Líquida , Feminino , Humanos , Limite de Detecção , Masculino , Espectrometria de Massas , Pessoa de Meia-Idade , Detecção do Abuso de Substâncias/métodos , Adulto Jovem
2.
Drug Test Anal ; 6(4): 367-75, 2014 Apr.
Artigo em Inglês | MEDLINE | ID: mdl-23868723

RESUMO

The range of novel psychoactive substances (NPS) including phenethylamines, cathinones, piperazines, tryptamines, etc. is continuously growing. Therefore, fast and reliable screening methods for these compounds are essential and needed. The use of dried blood spots (DBS) for a fast straightforward approach helps to simplify and shorten sample preparation significantly. DBS were produced from 10 µl of whole blood and extracted offline with 500 µl methanol followed by evaporation and reconstitution in mobile phase. Reversed-phase chromatographic separation and mass spectrometric detection (RP-LC-MS/MS) was achieved within a run time of 10 min. The screening method was validated by evaluating the following parameters: limit of detection (LOD), matrix effect, selectivity and specificity, extraction efficiency, and short-term and long-term stability. Furthermore, the method was applied to authentic samples and results were compared with those obtained with a validated whole blood method used for routine analysis of NPS. LOD was between 1 and 10 ng/ml. No interference from matrix compounds was observed. The method was proven to be specific and selective for the analytes, although with limitations for 3-FMC/flephedrone and MDDMA/MDEA. Mean extraction efficiency was 84.6 %. All substances were stable in DBS for at least a week when cooled. Cooling was essential for the stability of cathinones. Prepared samples were stable for at least 3 days. Comparison to the validated whole blood method yielded similar results. DBS were shown to be useful in developing a rapid screening method for NPS with simplified sample preparation.


Assuntos
Teste em Amostras de Sangue Seco/métodos , Psicotrópicos/sangue , Espectrometria de Massas em Tandem/métodos , Cromatografia Líquida/métodos , Humanos , Limite de Detecção
3.
Int J Legal Med ; 127(4): 769-75, 2013 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-23283405

RESUMO

BACKGROUND: Ethyl glucuronide (EtG) and ethyl sulfate (EtS) are non-oxidative minor metabolites of ethanol. They are detectable in various body fluids shortly after initial consumption of ethanol and have a longer detection time frame than the parent compound. They are regarded highly sensitive and specific markers of recent alcohol uptake. This study evaluates the determination of EtG and EtS from dried blood spots (DBS), a simple and cost-effective sampling method that would shorten the time gap between offense and blood sampling and lead to a better reflectance of the actual impairment. METHODS: For method validation, EtG and EtS standard and quality control samples were prepared in fresh human heparinized blood and spotted on DBS cards, then extracted and measured by an LC-ESI-MS/MS method. Additionally, 76 heparinized blood samples from traffic offense cases were analyzed for EtG and EtS as whole blood and as DBS specimens. The results from these measurements were then compared by calculating the respective mean values, by a matched-paired t test, by a Wilcoxon test, and by Bland-Altman and Mountain plots. RESULTS AND DISCUSSION: Calibrations for EtG and EtS in DBS were linear over the studied calibration range. The precision and accuracy of the method met the requirements of the validation guidelines that were employed in the study. The stability of the biomarkers stored as DBS was demonstrated under different storage conditions. The t test showed no significant difference between whole blood and DBS in the determination of EtG and EtS. In addition, the Bland-Altman analysis and Mountain plot confirmed that the concentration differences that were measured in DBS specimens were not relevant.


Assuntos
Consumo de Bebidas Alcoólicas/sangue , Análise Química do Sangue , Manchas de Sangue , Glucuronatos/sangue , Ésteres do Ácido Sulfúrico/sangue , Biomarcadores/sangue , Cromatografia Líquida , Toxicologia Forense/métodos , Humanos , Espectrometria de Massas , Manejo de Espécimes
4.
Dalton Trans ; (33): 6634-44, 2009 Sep 07.
Artigo em Inglês | MEDLINE | ID: mdl-19672508

RESUMO

Synthetic approaches to 6,6'-disubstituted-2,2'-bipyridine ligands bearing carboxylic acid substituents at the 4,4' or 5,5'-positions are described. Copper(I) complexes with these ligands have been prepared for use in copper-based dye-sensitized solar cells. The single-crystal structures of 6,6'-dimethyl-2,2'-bipyridine-4,4'-dicarboxylic acid (H(2)4), [H(3)6][CF3CO2].2CF3CO2H (H(2)6 = 6,6'-diphenyl-2,2'-bipyridine-4,4'-dicarboxylic acid) and 4[Cu(H(2)2)(H2)].3H2O (H(2)2 = 6,6'-dimethyl-2,2'-bipyridine-5,5'-dicarboxylic acid) are described, as well as those of the intermediates (1E,5E)-1,6-di(2-furyl)hexa-1,5-diene-3,4-dione and 4,4'-di(2-furyl)-6,6'-dimethyl-2,2'-bipyridine (3), and the copper(I) complex [Cu(3)(2)][PF6]. The roles that classical and non-classical hydrogen bonding and pi-stacking interactions play in determining the solid-state packing in these structures are discussed. Preliminary studies of DSCs with these complexes are reported.

5.
Chem Commun (Camb) ; (32): 3717-9, 2008 Aug 28.
Artigo em Inglês | MEDLINE | ID: mdl-18685754

RESUMO

Dye-sensitized solar cells with carboxylate-derivatized {Cu(I)L(2)} complexes are surprisingly efficient and offer a long-term alternative approach to ruthenium-functionalized systems.

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