A new approach to ion exchange chromatography with conductivity detection for adulterants investigation in dietary supplements.

The extent of adulteration of dietary supplements has significantly increased in recent years. This situation worries health authorities and requires auxiliary analytical tools for the investigation of illegal substances purposely added. Ion exchange chromatography with conductivity detection is a consolidated analytical technique for the determination of inorganic compounds in various matrices. This technique has been applied to the pharmaceutical characterization of mainly impurities and degradation products. This work presents a new approach to ion exchange chromatography as a screening method to investigate the presence of amfepramone, femproporex, sibutramine, bisacodyl and amiloride in dietary supplements advertised for weight loss. The method was optimized and validated using a Metrosep C4 100/4.0 cation exchange column. The mobile phase consisted of 1.8 mm HNO3 containing 2% acetonitrile (v/v), with a flow rate of 0.9 ml min-1 , and nonsuppressed conductivity detection was applied. The limits of detection and quantification varied from 1.01 to 3.62 mg L-1 and from 1.48 to 8.72 mg L-1 , respectively. The proposed method was successful applied to 78 solid dietary supplement samples, in two of which adulterations were found. Moreover, ion exchange chromatography with conductivity detection could be easily used for quality control without prior complex sample pre-treatment.

Regulatory framework for dietary supplements and the public health challenge.

OBJECTIVE: The new regulatory framework for dietary supplements in Brazil prompted this analysis of the current outlook of these products and the challenges posed by the new guidelines. METHODS: We conducted a qualitative, observational and descriptive study of dietary supplements commercialized in Brazilian online stores with the help of the Google® search tool. We considered the ingredients on the labels, the effects attributed to these products and the commercial claims used as a means of promoting them to assess the necessary changes for the legal framework in the new guidelines. Finally, with the help of a database, we compared the effects declared by the manufacturers and attributed to certain ingredients with the scientific evidence described in literature. RESULTS: In total, we purchased 44 dietary supplements from Brazilian online stores (n = 7). Of the samples studied, 34.2% could not be classified in the category Dietary Supplements, as recommended by the new regulation of the Brazilian Health Regulatory Agency due to the presence of prohibited substances; 16% of products should be commercialized as medicines. Regarding the commercial appeals, 97.7% had banned expressions. Numerous claims of effects attributed to certain products were characterized as consumer fraud because they have no scientific evidence. CONCLUSIONS: The necessary changes represent a major regulatory and production challenge due to the wide range of dietary supplements and markets, an effort that aims to protect the consumers' health. Some previous gaps in the regulatory framework were not fully solved.

Simultaneous determination of iron and nickel as contaminants in multimineral and multivitamin supplements by solid sampling HR-CS GF AAS.

A methodology to assay simultaneously iron and nickel present as contaminants in multimineral and multivitamin supplements was investigated. High-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sample analysis were used. Measurements were done with the secondary lines of Fe (352.604 nm) and Ni (352.454 nm) to avoid spectral interferences. The best temperatures for pyrolysis and atomization for Fe and Ni were 1000 and 2700 °C, respectively. Chemical modifiers were not necessary and no matrix effects were observed. Aqueous standard solutions were used for calibration. The limit of detection was 0.517 µg g-1 for Fe and 0.011 µg g-1 for Ni. The precision ranged from 4.3% to 17% and 4.4-20% for Fe and Ni, respectively. The method accuracy was confirmed by comparing statistically the results obtained by solid sampling with those of sample acid digestion. The proposed methodology was successfully applied to determine both metals in different multimineral and multivitamin supplements.

Determination of phenolic and triterpenic compounds in Jatropha gossypiifolia L by Ultra-high performance liquid chromatography-tandem mass spectrometric (UHPLC-MS/MS)

This work describes the chemical characterization of extracts of Jatropha gossypiifolia (from Amazonia region) concerning the presence of phenolic and triterpenic compounds using Ultra High Perfomance Liquid chromatography coupled to Mass Spectrometry in Tandem (UHPLC-MS/MS) methods. The studied compounds belong to the most frequently found classes in medicinal plants (triterpenes, flavonoids, flavones, hydroxycinnamic acids, coumarins, catechins and stilbenes), which have been analyzed as chemical and bioactive markers in hydroethanolic and aqueous extracts. Several polyphenolic compounds identified herein are unprecedented in the scientific literature for this species. The chemical markers identified and quantified in the studied extracts of J. gossypiifolia were gallic acid, chlorogenic acid, catechin, caffeic acid, vanillic acid, p-coumaric acid, ferullic acid, rutin, quercitrin, 3-acetylcoumarin, trans-cinnamic acid, quercetin, luteolin, apigenin, kaempferol, chrysin. α-amyrin, β-amyrin and lupeol. As the majority compounds, (+)-catechin, p-coumaric acid, ferulic acid, luteolin, α-amyrin and β-amyrin were found to be present at mg kg-1 levels. J. gossypiifolia extracts presented a high in vitro activity against different reactive oxygen species (hydroxyl, peroxyl, and superoxide anion radicals). Several polyphenolic compound data presented herein are unprecedented in the scientific literature for this plant species. As a result, this plant can be a new source of bioactive molecules for therapeutic purposes.

Regulatory framework for dietary supplements and the public health challenge / Marco regulatório dos suplementos alimentares e o desafio à saúde pública

ABSTRACT OBJECTIVE The new regulatory framework for dietary supplements in Brazil prompted this analysis of the current outlook of these products and the challenges posed by the new guidelines. METHODS We conducted a qualitative, observational and descriptive study of dietary supplements commercialized in Brazilian online stores with the help of the Google® search tool. We considered the ingredients on the labels, the effects attributed to these products and the commercial claims used as a means of promoting them to assess the necessary changes for the legal framework in the new guidelines. Finally, with the help of a database, we compared the effects declared by the manufacturers and attributed to certain ingredients with the scientific evidence described in literature. RESULTS In total, we purchased 44 dietary supplements from Brazilian online stores (n = 7). Of the samples studied, 34.2% could not be classified in the category Dietary Supplements, as recommended by the new regulation of the Brazilian Health Regulatory Agency due to the presence of prohibited substances; 16% of products should be commercialized as medicines. Regarding the commercial appeals, 97.7% had banned expressions. Numerous claims of effects attributed to certain products were characterized as consumer fraud because they have no scientific evidence. CONCLUSIONS The necessary changes represent a major regulatory and production challenge due to the wide range of dietary supplements and markets, an effort that aims to protect the consumers' health. Some previous gaps in the regulatory framework were not fully solved.

RESUMO OBJETIVO O novo marco regulatório para os suplementos alimentares no Brasil instigou a presente análise do panorama atual desses produtos e os desafios impostos pelas novas diretrizes. MÉTODOS Foi realizado um estudo qualitativo, observacional e descritivo dos suplementos alimentares comercializados em lojas virtuais brasileiras, com o auxílio da ferramenta de busca Google®. Os ingredientes declarados nos rótulos, bem como os efeitos atribuídos a esses produtos e as alegações comerciais utilizadas como forma de promovê-los foram levados em consideração a fim de avaliarmos as mudanças necessárias para o enquadramento legal nas novas diretrizes. Por fim, com o auxílio de base de dados, foram comparados os efeitos declarados pelos fabricantes e atribuídos a determinados ingredientes com as evidências científicas descritas na literatura. RESULTADOS No total, foram adquiridos 44 suplementos alimentares provenientes de lojas virtuais brasileiras (n = 7). Das amostras estudadas, 34,2% não poderiam ser enquadradas na categoria Suplementos Alimentares, conforme preconiza a nova regulação da Agência Nacional de Vigilância Sanitária, em decorrência de presença de substâncias não permitidas; 16% dos produtos deveriam ser comercializados como medicamentos. Quanto aos apelos comerciais, 97,7% apresentavam expressões não permitidas. Inúmeras alegações de efeitos atribuídos a determinados produtos, por não possuírem comprovação científica, foram caracterizadas como fraude contra o consumidor. CONCLUSÕES Dada a extensa gama de suplementos alimentares e pontos de comercialização, as mudanças necessárias representam um grande desafio regulatório e de produção, esforço este que visa a proteger a saúde dos consumidores. Algumas lacunas previamente existentes ao marco regulatório ainda não foram totalmente solucionadas.