RESUMO
A simple, fast and sensitive method for the determination of quetiapine in human blood has been developed and validated. The method involved a basic liquid-liquid extraction procedure and subsequent analysis by gas chromatography-mass spectrometry, previous derivatization with bis(trimethylsilyl)-trifluoro-acetamide and chorotrimethylsilane (99 : 1). The methods of validation included linearity with a correlation coefficient > 0.99 over the range 0.02-1 µg ml(-1), intra- and interday precision (always < 12%) and accuracy (mean relative error always < 12%) to meet the bioanalytical acceptance criteria. The limit of detection was 0.005 µg ml(-1). The procedure was further applied to post mortems from the Institute of Legal Medicine, University of Santiago de Compostela.
Assuntos
Antipsicóticos/sangue , Autopsia/métodos , Dibenzotiazepinas/sangue , Adulto , Idoso , Antipsicóticos/intoxicação , Calibragem , Dibenzotiazepinas/intoxicação , Feminino , Cromatografia Gasosa-Espectrometria de Massas , Cabelo/química , Humanos , Indicadores e Reagentes , Masculino , Pessoa de Meia-Idade , Fumarato de Quetiapina , Reprodutibilidade dos TestesRESUMO
The performance of microwave-assisted extraction and HPLC with photodiode array detection method for determination of six analgesic and anti-inflammatory drugs from plasma and urine, is described, optimized, and validated. Several parameters affecting the extraction technique were optimized using experimental designs. A four-factor (temperature, phosphate buffer pH 4.0 volume, extraction solvent volume, and time) hybrid experimental design was used for extraction optimization in plasma, and three-factor (temperature, extraction solvent volume, and time) Doehlert design was chosen to extraction optimization in urine. The use of desirability functions revealed the optimal extraction conditions as follows: 67°C, 4 mL phosphate buffer pH 4.0, 12 mL of ethyl acetate and 9 min, for plasma and the same volume of buffer and ethyl acetate, 115°C and 4 min for urine. Limits of detection ranged from 4 to 45 ng/mL in plasma and from 8 to 85 ng/mL in urine. The reproducibility evaluated at two concentration levels was less than 6.5% for both specimens. The recoveries were from 89 to 99% for plasma and from 83 to 99% for urine. The proposed method was successfully applied in plasma and urine samples obtained from analgesic users.
Assuntos
Analgésicos/isolamento & purificação , Anti-Inflamatórios/isolamento & purificação , Micro-Ondas , Analgésicos/sangue , Analgésicos/urina , Anti-Inflamatórios/sangue , Anti-Inflamatórios/urina , Cromatografia Líquida de Alta Pressão , Humanos , Espectrofotometria Ultravioleta , Propriedades de SuperfícieRESUMO
Robust and simple validated analytical methods are required in postmortem toxicology to confirm immunoassay screening analysis of drugs of abuse. In this work, microwave-assisted extraction (MAE) was evaluated as an alternative method for extraction of target compounds such as cocaine, benzoylecgonine, cocaethylene, morphine, codeine, 6-monoacetylmorphine, methadone, and 2-ethylidene-1,5-dimethyl-3,3-diphenylpyrrolidine from vitreous humor. The MAE procedure parameters, namely, extraction temperature, time, and solvent volume, were optimized using a central composite design and applying desirability functions. The optimal conditions for extraction were 80 °C, 8 min, and 15 mL of dichloromethane solvent. The MAE-high-performance liquid chromatography-diode-array detection method was validated, showing its capability for the detection of concentrations in the range from 33 to 76 ng mL(-1) and recoveries in the range from 87 to 99.3% for all drugs. The MAE-based method was tested for 15 vitreous humor samples from forensic cases and its performance was compared with that of a solid-phase extraction method previously developed by our group. In general, better recovery and precision were achieved with the use of the MAE-based procedure.