Espectrometria de massas ambiente e tandem na quantificação de drogas de abuso
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Data
2018-09-10
Autores
Santos, Heloa
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Universidade Federal do Espírito Santo
Resumo
Mass spectrometry (MS) is a powerful tool because has high resolution and specificity for molecules chemical characterization. Initially, paper chromatography was developed using Dragendorff reagent and paper spray ionization mass spectrometry (PS-MS) for quantification. Then, polymers with electrical conductivity (PC) were studied because they are promising in high voltage applied in PS-MS and charging drops formation. Furthermore, PC-coated paper surface can be determinant for analyzes of various analytes, such as: avermectins, bupropion and its metabolites, anesthetics, anxiolytics, hormones, meloxicam, adulterants and drugs of abuse. The emergence of new psychoactive substances (NPS) is worldwide and alarming. Considering this growing market for NPS synthesis, the last part of this study presents a simple direct analysis in real time (DART) method. In Chapter 2, The method presented linearity greater than 0.98 and LODs of 6.51 ?g/mL, 13.53 ?g/mL and 0.35 mg/mL for Cocaína, levamisole and Lidocaína, respectively. Ten samples were quantified by PS(+)-MS and there was not statistically significant difference between PS(+)-MS and gas chromatography with flame ionization detector (GC-FID) at a significance level of 5 %. In Chapter 3, Polypyrrole (PPy), Polyaniline (PAni) or both polymers [Poly (Py-co-Ani)] were synthetized on paper by in situ polymerization. All the analytes were tested by PS (+)-FT-ICR and, in most cases, coated papers showed a higher absolute intensity signal compared to conventional chromatographic paper. The [Poly (Py-co-Ani)] paper showed better results and the linearity of the response was evaluated in Orbitrap (r2> 0.9851). The [Poly (Py-co-Ani)] paper was subjected to the reuse test and, compared to the traditional chromatographic paper, its results are promising for qualitative and quantitative PS-MS analysis. In Chapter 4, preliminary screening with DART-MS accelerates the detection process for 25 compounds among the most prominent classes of NPS, including synthetic cannabinoids and cathinone derivatives. Methanolic extracts were studied by DART(+)-MS/MS and it was efficient for rapid screening and detection of NPS in oral fluid and the herbal material (Turnera diffusa). LC-MS was able to generate MS/MS spectra with adequate linearity and sensitivity. The method was fully validated in the range of 0.01 to 100 ppb. Preliminary result of proposed off-line SPE protocol showed acceptable recoveries for the majority of drugs. Quality control samples were used during the method validation process, and all analytes showed RSD below 20 %
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Espectrometria de massa , Cromatografia em papel , Polímeros condutores