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Techniques for Extraction of Brewer’s Spent Grain Polyphenols: a Review

Publication . Guido, Luis F.; Moreira, Manuela M.

Million tons of brewer’s spent grain (BSG) are annually produced worldwide as brewing industry by-products. BSG represents a valuable source of phenolic compounds, which have attracted much attention due to their diverse health benefits. Relevant strategies have been developed for their efficient extraction, in order to commercially exploit these resources. This review focuses on the current extraction methods used to obtain phenolic compounds from BSG, ranging from more traditional to advanced techniques. The commonly used methods are the conventional solid–liquid extractions, employing organic solvents, alkaline, and enzymatic reactions. However, the inherent difficulties in screening and obtaining these compounds have led to the development of advanced extraction techniques. Pressurized fluid extraction, supercritical extractions, and microwave-assisted and ultrasound-assisted extractions are some of the novel extraction techniques that have been recently explored. These techniques have been mostly applied for phenolic recovery from barley and malt, as well as other types of cereals. In this review, it is shown that these novel techniques may provide an innovative approach to extract phenolics from BSG or related products, following an in-depth discussion on the major strengths and weaknesses identified in each technique.

2017Journal article

Open access

Dual-function hydrotalcite-derived adsorbents with sulfur storage properties: Dyes and hydrotalcite fate in adsorption-regeneration cycles

Publication . Stawiński, Wojciech; Węgrzyn, Agnieszka; Freitas, Olga; Chmielarz, Lucjan; Figueiredo, Sónia

Thermal treatment of hydrotalcite at increasing temperatures resulted in formation of mixed oxides that exhibited different adsorption behavior toward anionic and cationic industrial dyes. The material annealed at 450 °C was characterized by the highest maximum adsorption capacity for both types of dyes. The adsorption was strongly pH dependent and for the anionic dye abatement low pH was favored whilst higher pH was more preferable for removal of the cationic dye. According to the equilibrium experiments, the maximum adsorption capacity increased from 179 ± 5 to 291 ± 8 mg g−1 in case of the anionic dye at pH 3.5 and from 6 ± 2 to 48 ± 2 mg g−1 in case of the cationic dye at pH 8.0, on starting and thermally treated material at 450 °C, respectively. Detailed characteristics of spent adsorbent and its reconstructed form revealed that after each cycle of adsorption and thermal regeneration the maximum adsorption capacity of the material decreased due to changes in the structure and accumulation of sulfur compounds. Evolution of specific surface area and porosity was correlated with annealing temperatures and behavior of dye's residues.

2017Journal article

Open access

Analysis of pharmaceutical adulterants in plant food supplements by UHPLC-MS/MS

Publication . Paíga, Paula; Rodrigues, Manuela J.E.; Correia, Manuela; Amaral, Joana S.; Oliveira, M. Beatriz P.P.; Delerue-Matos, Cristina

A method based on the Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) extraction and ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS) was successfully developed and validated for the analysis of 26 pharmaceutical compounds belonging to different therapeutic classes (anorexics, stimulants, anxiolytics, antidepressants and laxatives), which are all prone to be illegally added into weight-loss plant food supplements (PFS) for their pharmacological activity. Internal standard calibration with six isotopically labelled compounds rendered good linearity in the range of 5 to 1000μg/l, depending on the compound, and good sensitivity with limits of quantification in the range of 0.02-9.80μg/l. Recoveries were assessed for all the 16 samples analysed and were found between 70% and 120% for over 90% of the analytes. The average recovery value was 90.8%, for the different studied matrices (liquids, liquid ampoules, tablets and capsules), with RSD values lower than 10% for all forms. The changes introduced to the QuEChERS procedure maintained the good performance characteristics of the extraction method while preserving the chromatographic system for the introduction of unwanted matrix compounds. Synephrine was the only compound detected and quantified in one sample, but at a very low concentration (768μg/l) and its presence may be due to the plant extracts used in the formulation, as synephrine is known to be a natural constituent of Citrus aurantium amara. Despite none of the 16 evaluated samples were found to be adulterated by the illegal addition of the drugs included in this work, the developed methodology can be very useful for monitoring the adulteration of weight-loss PFS.

2017Journal article

Open access

Acid-base treated vermiculite as high performance adsorbent: Insights into the mechanism of cationic dyes adsorption, regeneration, recyclability and stability studies

Publication . Stawiński, Wojciech; Węgrzyn, Agnieszka; Dańko, Tomasz; Freitas, Olga; Figueiredo, Sónia; Chmielarz, Lucjan

Additional treatment with NaOH of acid activated vermiculite results in even higher increase in the adsorption capacity in comparison to samples modified only in acidic solution (first step of activation) with respect to raw material. Optimization of treatment conditions and adsorption capacity for two cationic dyes (methylene blue (MB) and astrazon red (AR)), also as binary mixture, was evaluated. The capacity, based on column studies, increased from 48 ± 2 to 203 ± 4 mg g-1 in the case of methylene blue and from 51 ± 1 to 127 ± 2 mg g-1 in the case of astrazon red on starting and acid-base treated material, respectively. It was shown that adsorption mechanism changes for both cationic dyes after NaOH treatment and it results in decrease of adsorption rate. In binary mixtures methylene blue is bound stronger by adsorbent and astrazon red may be removed in initial stage of adsorption. Extensive studies on desorption/regeneration process proved high efficiency in recyclable use of all materials. Although cation exchange capacity decreases due to acid treatment, after base treatment exchange properties are used more efficiently. On the other hand, increased specific surface area has less significant contribution into the adsorption potential of studied materials. Obtained adsorbents worked efficiently in 7 adsorption-regeneration cycles and loss of adsorption capacity was observed only in two first cycles.

2017Journal article

Open access

A factorial design for optimization of the analytical variables on the development of a genoassay for the transgenic soybean detection

Publication . Ramos-Jesus, J.; Barroso, M. Fátima; M. S. Silva, Luís; Pereira, C.; Freire, C.; de-los- Santos-Álvarez, N.; Leite, José Roberto S.A.; Delerue-Matos, Cristina

At the laboratory, analytical method optimizations are performed to achieve the maximum sensitivity and selectivity. Routinely, this procedure is carried out by optimizing one-factor-at-a-time approach until there is no further improvement, where each experimental parameter is optimized separately and independently of the other factors.

2015Conference object

Open access