RESUMEN
The 22 amphetamine-derived synthetic drugs (ADSDs), mostly cathinones, were examined by gas chromatography with mass spectrometry using two different derivatization methods with (i) heptafluorobutyric anhydride (HFBA) and (ii) pentafluorobenzoyl chloride (PFBCl). Both developed derivatization approaches were evaluated and compared for urine and serum samples. Extraction procedures proved to give satisfactory results with regard to recoveries and extract purity, even though both derivatization methods reached acceptable sensitivity for the intended use. The derivatization with PFBCl showed better results with respect to retention and response stability, thus the PFBCl method was selected for validation. Calibration curves were linear over the tested concentration range of 20-1,000 ng/mL with the R(2) values ranging from 0.994 to 0.998. Intra- and interday precisions and accuracies were within 20% for all concentrations in the linear range. The limit of detection was determined to be lower than 2 ng/mL for all 22 analytes. The method proved to be a useful analytical tool in the course of systematic toxicological analysis.
Asunto(s)
Anfetaminas/análisis , Drogas de Diseño/análisis , Cromatografía de Gases y Espectrometría de Masas , Detección de Abuso de Sustancias/métodos , Anfetaminas/sangre , Anfetaminas/orina , Métodos Analíticos de la Preparación de la Muestra , Benzoatos/química , Calibración , Fluorocarburos/química , Humanos , Límite de Detección , Sensibilidad y EspecificidadRESUMEN
Synthetic cannabinoids have gained popularity due to their easy accessibility and psychoactive effects. Furthermore, they cannot be detected in urine by routine drug monitoring. The wide range of active ingredients in analyzed matrices hinders the development of a standard analytical method for their determination. Moreover, their possible side effects are not well known which increases the danger. This review is focused on the sample preparation and the determination of synthetic cannabinoids in different matrices (serum, urine, herbal blends, oral fluid, hair) published since 2004. The review includes separation and identification techniques, such as thin layer chromatography, gas and liquid chromatography and capillary electrophoresis, mostly coupled with mass spectrometry. The review also includes results by spectral methods like infrared spectroscopy, nuclear magnetic resonance or direct-injection mass spectrometry.
Asunto(s)
Cannabinoides/análisis , Técnicas de Química Analítica/métodos , Drogas de Diseño/análisis , Animales , Cannabinoides/metabolismo , Cannabinoides/farmacocinética , Cannabinoides/farmacología , Técnicas de Química Analítica/instrumentación , Cromatografía Liquida/instrumentación , Cromatografía Liquida/métodos , Cromatografía en Capa Delgada/instrumentación , Cromatografía en Capa Delgada/métodos , Drogas de Diseño/metabolismo , Drogas de Diseño/farmacocinética , Drogas de Diseño/farmacología , Electroforesis Capilar/instrumentación , Electroforesis Capilar/métodos , Humanos , Espectrometría de Masas/instrumentación , Espectrometría de Masas/métodos , Extracción en Fase Sólida/instrumentación , Extracción en Fase Sólida/métodosRESUMEN
The CE-ESI-MS/MS method for the identification, separation and determination of mushroom toxins, namely ibotenic acid, muscimol and muscarine, was developed. It proved to be sensitive and thus useful for the real sample analysis with omitting the labor and time consuming pretreatment step. The CE-ESI-MS/MS method was applied on the spiked human urine. The analytical characteristics of the proposed method, such as limits of detection, linearity and repeatability of the peak area and the migration time, were evaluated. The RSD of the migration time and peak area were from 0.93% to 1.60% and from 2.96% to 3.42%, respectively. The obtained LOD values were at the nanomolar concentration level, therefore the developed method is sufficient for the determination and quantification of studied toxins in human urine after mushroom intoxication.
Asunto(s)
Agaricales/química , Ácido Iboténico/análisis , Muscarina/análisis , Muscimol/análisis , Intoxicación por Setas/orina , Urinálisis/métodos , Electroforesis Capilar , Humanos , Ácido Iboténico/orina , Límite de Detección , Muscarina/orina , Muscimol/orina , Ósmosis , Reproducibilidad de los Resultados , Espectrometría de Masa por Ionización de Electrospray , Espectrometría de Masas en TándemRESUMEN
Some methodological aspects of an on-line combination of capillary zone electrophoresis with mass spectrometric detection (CZE-QqQ-MS) were studied in this work as well as the possibilities of using this combination for analysis of the high-molecular mass compounds present in multi-component matrices. All experiments using an on-line combination of capillary electrophoresis with mass spectrometric detection were carried out in cationic mode in covalently-coated capillary. The optimised electrolyte system consisted of 100 mmol/L formic acid. Prior to the CZE-QqQ-MS analysis, an extraction of lysozyme from cheese samples using 1 mol/L of acetic acid was performed. The LOD was 3.6 mg lysozyme per kg and the LOQ was 10.9 mg lysozyme per kg. The concentration range of the lysozyme determined in four cheese samples analysed in this work was from 0.5 to 3.3g of lysozyme per kg. The values of the relative standard deviations thus obtained were from 4.6% to 9.3% depending on the cheese sample.
Asunto(s)
Queso/análisis , Proteínas del Huevo/análisis , Electroforesis Capilar/métodos , Conservantes de Alimentos/análisis , Espectrometría de Masas/métodos , Muramidasa/análisis , Animales , PollosRESUMEN
A screening analytical method based on an automated on-line combination of capillary isotachophoresis-capillary zone electrophoresis (cITP-CZE) in hydrodynamically closed separation system, equipped with photometric detection at 280 nm, was developed for a routine determination of the selected biogenic amines, namely histamine, 2-phenylethylamine and tyramine, in red wines. The evaluated limits of detection (LODs) were 0.35 mg L(-1) for histamine, 0.33 mg L(-1) for 2-phenylethylamine and 0.37 mg L(-1) for tyramine. The repeatability of the migration time and peak area for histamine were 1.1% and 2.6%, respectively, for 2-phenylethylamine 0.7% and 2.0%, respectively, and for tyramine 0.8% and 2.1%, respectively. The method recoveries were 92.1% for histamine, 96.4% for 2-phenylethylamine and 95.5% for tyramine. The developed automated cITP-CZE-UV method was applied for the determination of histamine, 2-phenylethylamine and tyramine in seven red wine samples originating from Czech Republic.