RESUMO
The toxic Paraphenylenediamine is characterized by infrared spectrophotometry and nuclear magnetic resonance spectroscopy, whereas, high performance liquid chromatography with a refractive index detector was used to determine its purity in the suspect samples using external standardisation. An analytical method for determination of lower traces of paraphenylenediamine in post-mortem biological fluids was developed. This procedure involves deproteneization or hydrolysis followed by liquid-liquid extraction and derivatization with trifluoroacetic anhydride. 1 microL of the extract was then analysed by gas chromatography/iontrap mass spectrometry. Benzidine used as the internal standard for quantification and the extraction recovery test was evaluated to 85%. This method was validated in cases with paraphenylenediamine poisoning.
Assuntos
Fenilenodiaminas/sangue , Fenilenodiaminas/urina , Adolescente , Adulto , Feminino , Humanos , Fenilenodiaminas/intoxicaçãoRESUMO
In this study, we describe a HS-GC/MS method as a new analytical technique for the detection of triacetone triperoxide (TATP) traces in samples from post-explosion debris. We evaluate the optimum parameters for the analysis of this product with lowliness thermal decomposition and for the detection of TATP lesser than nanogram (.1 ng) level.
RESUMO
A method for qualitative and quantitative determination of paraphenylenediamine in biological fluids (blood, urine and gastric content) was developed. This analytical procedure involves deproteneisation or hydrolysis, liquid-liquid extraction, derivatization with TFA followed by GC-MS iontrap analysis. Benzidine was the internal standard used for quantification and the extraction recovery test was about 85%. The detection limit of paraphenylenediamine was determined at 0.1 pg (S/N=10).