Liquid chromatographic determination of caffeine and adrenergic stimulants in food supplements sold in Brazilian e-commerce for weight loss and physical fitness

Methyl-xanthines and adrenergic stimulants, such as caffeine and synephrine, are commonly added to food supplements due to their stimulating and thermogenic effects. In addition, the abusive consumption of food supplements with ergogenic and aesthetic purposes has been observed worldwide. This work describes the study of caffeine, p-synephrine, hordenine, octopamine, tyramine, ephedrine and salicin as stimulants in dietary supplements marketed in Brazil for weight loss and physical fitness claims. A total of 94 different products were acquired from 30 Brazilian websites. Thus, the sampling of marketed supplements was performed in virtual commerce (e-commerce) with claims of weight loss, appetite reduction, fat burning and metabolism acceleration. The developed analytical method involved the separation of the stimulants by HPLC with diode array detection (HPLC-DAD) by using a gradient elution of flow rate (0.7–2.5 ml min^?1) and mobile phase composition (0.1% H₃PO₄/methanol). The validated method was applied to the study of 46 dietary supplements. Caffeine, p-synephrine and ephedrine were found to be present as stimulants in 52% of the studied samples marketed as encapsulated or bulk forms. Caffeine was found to be present in concentrations that represent doses from 25.0 to 1476.7 mg day^–1. Synephrine was found in concentrations that represent doses from 59.1 to 127.0 mg day^–1. Ephedrine was found to be associated with caffeine in one formulation at a concentration representing a 26.1 mg day^–1 dosage.     

Microencapsulation of cashew apple (Anacardium occidentale,L.) juice using a new chitosan–commercial bovine whey protein isolate system in spray drying

The aim of this work was to obtain a new stable food product from cashew apple juice encapsulated by spray-drying technique using chitosan–whey protein isolate systems. The materials were evaluated according to their physicochemical stability during storage at different conditions and characterized with respect to their particle size distribution and structure. Encapsulated commercial and natural juices showed homogenous and unimodal particle size distribution with diameters ranging from 0.2 to 5.0 μm and from 0.2 to 40.0 μm, respectively. Both juices demonstrated higher physicochemical stability for vitamin C and color measurements than their respective non-encapsulated juices. X-ray diffractograms evidenced that the powder juices after the 140th day of storage were still in amorphous state. These results indicate that the new product was effective in protecting sensitive compounds present in the food matrix and it was also able to remain stable throughout the study period.     

Dissolving grade eco-clean cellulose pulps by integrated fractionation of cardoon (Cynara cardunculus L.) stalk biomass

A biorefinery scheme with separate processing of the two main carbohydrate streams (cellulose and hemicellulose-derived) was employed to the energy crop cardoon (Cynara cardunculus L.) to fractionate the whole stalk material. A high quality xylose-enriched substrate was obtained after selective one-step dilute sulfuric acid hydrolysis of hemicelluloses, yielding 18.1 g of xylose per 100 g of dry biomass. The xylan-free solid residue was delignified by sulfur-free organosolv pulping to produce dissolving grade pulps having 93.8% of α-cellulose (33.1 g per 100 g dry initial biomass) and 79.5% degree of crystallinity. About 76% of crop lignin (13.8 g per 100 g dry initial biomass) was recovered from the spent pulping liquor as a high purity reactive precipitated organosolv lignin. Response surface methodology was used for statistical modeling and optimization of the applied separation processes. The central composite rotatable design was applied to assess the effects of the principal technological parameters on the main reaction outputs.     

Determining adulteration of canned products using SNIF-NMR and IRMS: detection of undeclared addition of synthetic acetic acid

Possible adulteration of canned products containing spirit vinegar pickle by adding synthetic acetic acid is a significant problem of the food industry. Isotope analyses, which determine botanical origin of acetic acid and also can detect synthetic acid, were applied to detect undeclared addition of synthetic acetic acid to canned products. The aim of the study was to improve the extraction technique for the SNIF-NMR (²H/¹H; site-specific natural isotopic fractionation-nuclear magnetic resonance) and IRMS (¹³C/¹²C; isotope ratio mass spectrometry) isotope methods and for an atypical matrix and to determine isotope ratios in canned vegetables pickle to prove their adulteration or authenticity. The following set of canned products was analysed: pickled cucumbers (n = 16) and one vinegar pickle purchased in the Czech market and six model (cucumber) pickles. The determined ratios of ²H/¹H and ¹³C/¹²C for the pickled cucumbers proved to be authentic ranged from 89.4 to 107.0 ppm and from ?28.7 to ?15.6 ‰, respectively; for the synthetic acetic acids diluted with water they ranged from 114.2 to 129.0 ppm and from ?44.9 to ?33.4 ‰, respectively. Isotope analyses were confirmed as a reliable tool for assessing authenticity of canned products. The method enables detection of synthetic acetic acid addition into vinegars and canned vegetables containing vinegar pickle up from 20 % (of total acidity).