ABSTRACT
A adição fraudulenta de ativos farmacêuticos em suplementos nutricionais é um problema mundial. É comum encontrar mensagens sobre perda de peso, aumento da capacidade intelectual e/ou física, e estímulo sexual na embalagem de suplementos adulterados com fármacos sintéticos ocultos em formulações aparentemente inofensivas para os usuários. No Brasil, a disponibilidade de dados sobre a adulteração de suplementos nutricionais é escassa. No presente trabalho, foi desenvolvido e aplicado um método analítico empregando cromatografia gasosa com detector de nitrogênio fósforo (GC-NPD) para a detecção, identificação e quantificação de estimulantes/anorexígenos não declarados nos rótulos de suplementos alimentares, tais como: cafeína, femproporex, anfepramona, fenfluramina, sibutramina, fentermina, efedrina, fenilpropanolamina, pseudoefedrina e 4- metilhexan-2-amina. A técnica de extração/solubilização com metanol foi utilizada, ressaltando a utilização de baixa quantidade de amostra, solvente e padrões de estimulantes. Após o desenvolvimento e validação do método, as análises foram aplicadas em amostras de suplementos nutricionais obtidos em lojas especializadas em suplementos, de diversas partes do estado de São Paulo (n=125). Das 125 amostras de suplemento nutricional analisadas, 38 delas (30%) apresentaram resultado positivo para alguma das substâncias de interesse, dentre elas, sibutramina, cafeína e efedrina mediante a metodologia escolhida. As amostras positivas foram posteriormente analisadas qualitativamente por LC-MS/MS, no propósito de confirmar o resultado positivo obtido. A técnica analítica empregada proporciona seletividade, linearidade, precisão, exatidão, recuperação e limites em conformidade ao objetivo que foram destinadas. Os métodos de preparo de amostra desenvolvidos e validados demonstraram ser simples, práticos, eficientes e diferenciados pelo baixo uso de amostra e solvente
The fraudulent addition of active pharmaceutical compounds in nutritional supplements is, indeed, a worldwide problem. Often, it can be found several advertisements on various supplement packaging assuring weight loss, increased intellectual and/or physical capacity and sexual stimulation. These products may have been 'spiked' with synthetic drugs containing formulations which are apparently harmless to users. In Brazil, the availability of data about adulteration of nutritional supplements is scarce. In the present work, an analytical method using gas chromatography coupled with a nitrogen-phosphorus detector (GC-NPD) was developed and applied for the detection, identification and quantification of undeclared stimulants and/or anorectic agents in food supplement labels, such as: caffeine, fenproporex, amfepramone, fenfluramine, sibutramine, phentermine, ephedrine, phenylpropanolamine, pseudoephedrine e 4- metilhexan -2- amine. The extraction/solubilization with methanol presented satisfactory results, emphasizing the use of low amount of sample, solvent and standards of analytes. After the development and validation, the method was applied in samples of nutritional supplements obtained from specialty stores in various parts of the state of São Paulo (n = 125). From the 125 nutritional supplement samples analyzed, 38 of them (30%) presented positive results for some of the substances of interest, among them sibutramine, caffeine and ephedrine according to the chosen methodology. The positive samples were subsequently analyzed qualitatively by LCMS / MS, in order to confirm the positive result obtained. The analytical technique employed provides selectivity, linearity, precision, accuracy, recovery and limits in accordance with the intended purpose. The sample preparation methods developed and validated to be simple, practical, efficient and differentiated by the low sample and solvent usage
Subject(s)
Laboratory and Fieldwork Analytical Methods/methods , Dietary Supplements/analysis , Appetite Depressants/administration & dosage , Drug ContaminationABSTRACT
A method has been developed for the determination of stimulants in products of nutritional supplement. The stimulants in the samples were extracted with a solution of sodium hydroxide and then cleaned up by liquid -liquid partitioning.The extracted stimulants were analyzed by gas chromatography with HP-5capilary column and detected by the Nitrogen-Phosphorus detector (NPD). The results showed that the method had good purifying effect with high sensitivity. The operation was also simple and quick. The detection limit ranged from 5 to 40 ?g/L and the average recovery rate was 75.4%～143.1% with relative standard deviations (RSDs) ranged from 0.27% to 5.5%.
ABSTRACT
urine.Conclusion The metabolism of MAP in animals tissues and body fluids is related to the time elapsed after guinea pigs death.