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Certified reference materials (CRM) of amphetamine derivatives were produced through a simple, rapid and efficient synthesis in both batch and continuous-flow conditions, accompanied by the development of a comprehensive certification protocol for this class of substances. Our chemistry enabled the synthesis of MDA, MDMA, PMA and PMMA in two steps from safrole and estragole with overall yields of 38-61 % in 48â hours under batch conditions and 61-65 % in 65â minutes under continuous-flow conditions, followed by the development of a certification protocol for these materials through identity checking, homogeneity, stability, and characterization studies. Furthermore, as result of this work, a very pure CRM of MDA.HCl with 99.1±1.4â g/100â g of certified characterization value was produced. Considering the importance of supplying amphetamine calibrants for public security efforts in Forensic Chemistry, the potential therapeutical applications, and responding to the rising demand for the synthesis of CRM, this work presents a pioneering approach for the production of amphetamine and related compounds.
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Usually, if percutaneous absorption tests are conducted in accordance with OECD Guideline 428, in vitro determination is accepted by mainly regulatory agencies. In this paper, we focus on the lack of comparability of the results regarding the permeation parameter/flow rate, although it is widely discussed in the literature. This work sought to evaluate the absorption of caffeine using Franz-type diffusion cell with porcine ear skin samples, varying the storage duration and the way to handle them. Metrological tools were used for caffeine quantification such as certified reference material candidate, calibrated instruments, and validated methodology. Our results corroborate with the recommendation that membranes should be freshly prepared or frozen for short periods. Samples frozen for approximately one year should not be used because they present high cutaneous absorption. The results obtained for the absorption rate (J) are comparable to the results obtained by previous studies using similar experimental conditions. The evidence of the barrier characteristic promoted by the stratum corneum and the effect promoted by the storage time is shown through J = 6.25 ± 0.48 µg/cm2/h. We demonstrated the importance of metrological tools to guarantee reproducibility and comparability of the results between different laboratories.
Assuntos
Cafeína , Organização para a Cooperação e Desenvolvimento Econômico , Animais , Epiderme/metabolismo , Reprodutibilidade dos Testes , Pele/metabolismo , Absorção Cutânea , SuínosRESUMO
Background: Coffee is an important agricultural commodity with technical barriers for exportation because of possible contamination with ochratoxin A (OTA), a mycotoxin nephrotoxic and carcinogenic. The maximum limit for OTA in roasted coffee is 5.0 µg/kg in the European Union and 10 µg/kg in Brazil, and the use of certified reference materials (CRM) is required for reliable measurements. Objective: This paper describes the development of a candidate CRM of OTA in roasted coffee following the requirements of ISO 17034 and ISO Guide 35. Methods: A primary method of isotope dilution MS was developed and validated using (13C20)-OTA as internal standard. The sample preparation was based on AOAC Official Methods of AnalysisSM using immunoaffinity column. Results: The linear working range is 2.0-15.0 µg/kg, with recoveries of 92.2-110.8% and relative SDs lower than 12.4%. The method was successfully applied to the feasibility study, which defined the procedure for preparation of a large batch around 5 µg/kg. It was produced by spiking blank roasted coffee with OTA standard, mixing and filling in amber flasks with 50 g of coffee, and storing at -80°C. The homogeneity study showed an acceptable degree of heterogeneity of 1.44%, and the short-term-stability study defined the conditions for transportation as maximum temperature of 50°C up to 28 days. Conclusions: These results show that certification is possible. Highlights: The long-term stability study at -20°C is in progress, and the characterization will be conduzed by a interlaboratory comparison. This material will be an important tool for QC in laboratories.