Alcohol is the most frequently abused 'addictive substance' that causes serious social problems throughout the world; thus alcoholism is of particular interest in clinical and forensic medicine. Ethyl glucuronide (EtG) is a marker of recent alcohol consumption that detects alcohol use reliably over a definite time period. The present paper describes a new method for the determination of EtG in urine. It was based both on microwave assisted extraction (MAE) to extract the analyte from urine samples, and gas chromatography-mass spectrometry (GC-MS) to identify and quantify the EtG in selected ion monitoring (SIM) mode. The method was applied to 33 urine samples from alcohol users, obtaining positive results in all cases. It was fully validated including a linear range (0.1-100 microg ml(-1)) and the main precision parameters. In summary, the use of microwave assisted extraction turned out to be a substantially simpler, faster and more sensitive procedure than any other conventional sample preparations.
Although blood is often used to detect and quantify the presence of drugs, there are some instances where samples obtained from other biological matrices, like pericardial fluid (PF), are necessary since adequate blood samples may not be available. PF is an epicardial transudate, which contains plasma components that include toxicological substances making this sample useful when blood samples are not available. This fluid is a well-preserved postmortem sample and can easily be collected in larger amounts without significant contamination, compared with other body fluids. Although studies involving PF began around the 1980s, the adequacy of such fluid as a biological matrix has been poorly investigated. Antidepressants are frequently detected in postmortem samples from forensic cases. Nowadays, they constitute some of the most commonly prescribed drugs worldwide. A total of seven antidepressants (venlafaxine, mirtazapine, olanzapine, paroxetine, sertraline, fluoxetine and citalopram) were evaluated in this study. A new extraction method involving dispersive liquid–liquid microextraction (DLLME) is presented in which chloroform and acetonitrile are determined to be the best extraction and dispersing solvents. The experimental design was achieved using StatGraphics 18. The response surface methodology enabled us to know the optimal volume for the two solvents used in the DLLME. The detection technique used was gas chromatography–mass spectrometry with electron impact ionization as ionization source. A temperature gradient has been used and the total chromatographic separation time was 19.43 min. Validation results met the international validation guidance (Food and Drug Administration (FDA)). Under the optimal condition, the method offered good validation parameters showing a new efficient, simple, rapid and sensitive method. The analytical method was applied to 31 PF samples. Twenty-one samples were positive with concentrations between 0.19 and 8.48 µg/mL. Venlafaxine and olanzapine were the antidepressants most frequently found.
A spectrophotometric method for the determination of hydrogen cyanide in biological fluids based on the release of cyanide ion by the addition of a strong acid and its subsequent specific reaction with hydroxocobalamin to give cyanocobalamin is proposed. The release of cyanide ion is accelerated by aeration with a stream of an inert gas (nitrogen) that carries it into the hydroxocobalamin solution. Although the in vitro reaction develops to completion within 20 min, reproducible quantitation in biological media takes 45 min. The cyanocobalamin formed is quantitated by second-derivative visible spectrophotometry from the absorbance difference between 333 and 361 nm, the measured signal being proportional to the cyanide ion concentration in the sample.
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