HS-SPME Gas Chromatography Approach for Underivatized Acrylamide Determination in Biscuits.

Acrylamide (AA) is a food contaminant in thermally processed products that is object of tight control. A simple and easy-to-apply methodology for routine monitoring of AA levels in food products could allow producers to be players in the control of their own products. In this work, a simple methodology for AA quantification without derivatization was developed for biscuits, for which the benchmark levels recommended by EFSA are 350 µg/kg, and 150 µg/kg for biscuits for infants and young children. Headspace-solid phase microextraction (HS-SPME) was used in 120 mL screwed-cap vials with a carboxen/polydimetylsiloxane fiber, 4 g of biscuits, and 10 mL of water during 15 min at room temperature under stirring. The addition of 30 mL of propanol under stirring during 15 min at room temperature and 15 min at 60 °C was used to promote AA transfer to the headspace. The fiber exposure was 45 min. A gas chromatography-mass spectrometry analysis allowed to obtain an external calibration curve at m/z 71, with linearity R2 > 0.99 and precision RSD < 9%. The detection and quantification limits were 27.4 µg/kg and 91.5 µg/kg, respectively. The methodology was successfully used in biscuits with lower AA amount, where mitigation strategies (asparaginase or pectate) were applied.

Microwave hydrodiffusion and gravity as a sustainable alternative approach for an efficient apple pomace drying.

Apple pomace valuation has been impaired by its high perishability and absence of fast drying approaches demanded by industry. This work aimed to assess the feasibility of Microwave Hydrodiffusion and Gravity (MHG) process applied for apple pomace drying using discrete delivery powers (300-900 W) and comparison with hot-air drying (40-100 °C). To dry 0.4 kg of apple pomace (81% moisture), hot-air drying required 3.6-9.9 h with estimated water evaporation flux of 1.0-3.5 mL/min. For MHG, which processed 1.2 kg, these corresponded to 1.0-2.6 h and 5.1-13.9 mL/min. Furthermore, MHG allowed water recovery containing part of apple pomace phenolic compounds and carbohydrates. The dried pomace was stable for 2 years, after which phenolic compounds and polysaccharides were still recoverable by hot water extractions. These results pave the way for MHG to be used for apple pomace and other by-products preservation, boosting their conversion into valuable co-product for valuation of its components.

Impact of microwave-assisted extraction on roasted coffee carbohydrates, caffeine, chlorogenic acids and coloured compounds.

Microwave-assisted extraction (MAE) allows to quickly achieve soluble compounds from solid matrices due to the promotion of temperatures higher than the solvent (atmospheric) boiling point, once a closed-vessel system is used for operating at high pressure. In this study, the feasibility of MAE for producing high yield coffee extracts with properties that allow their commercial application was tested through a quality by design approach. It was studied the influence of time of extraction (1, 5.5, 10 min), temperature (120, 150, 180 °C) and the mass-to-volume (m/V) ratio (2, 4, 6 g/60 mL) in the overall extraction yield (24-47%, w/w), carbohydrates content (18-43%, w/w), sugars composition, caffeine (4-7%, w/w), 5-caffeoylquinic acid (1-2%, w/w), colour and antioxidant activity of the extracts. FTIR analysis was used to study the resemblance of coffee extracts and commercial instant coffee. MAE allowed overall extraction yields considerably higher than the home brewing methods, mainly when performed at 180 °C, with a substantial increase in arabinogalactans (AG) extraction associated to higher temperatures. Temperature exerted a crucial role in coffee extracts differentiation, although time and m/V ratio also lead to different values in the responses. Under a circular economy concept, MAE was able to produce extracts that can be used as defined food/brew ingredients and provides a galactomannan and cellulose rich residue that can also be valued as a source of dietary fibre.

Apple Pomace Extract as a Sustainable Food Ingredient.

Apple pomace is a by-product of apple processing industries with low value and thus frequent disposal, although with valuable compounds. Acidified hot water extraction has been suggested as a clean, feasible, and easy approach for the recovery of polyphenols. This type of extraction allowed us to obtain 296 g of extract per kg of dry apple pomace, including 3.3 g of polyphenols and 281 g of carbohydrates. Ultrafiltration and solid-phase extraction using C18 cartridges of the hot water extract suggested that, in addition to the apple native polyphenols detected by ultra-high-pressure liquid chromatography coupled to a diode-array detector and mass spectrometry UHPLC-DAD-ESI-MSn, polyphenols could also be present as complexes with carbohydrates. For the water-soluble polyphenols, antioxidant and anti-inflammatory effects were observed by inhibiting chemically generated hydroxyl radicals (OH•) and nitrogen monoxide radicals (NO•) produced in lipopolysaccharide-stimulated macrophages. The water-soluble polyphenols, when incorporated into yogurt formulations, were not affected by fermentation and improved the antioxidant properties of the final product. This in vitro research paves the way for agro-food industries to achieve more diversified and sustainable solutions towards their main by-products.

Structural polymeric features that contribute to in vitro immunostimulatory activity of instant coffee.

An instant coffee fraction, rich in arabinogalactans, obtained by ultrafiltration, using 1 and 5kDa membranes, has previously shown in vitro stimulatory activity on BALB/c mice spleen B lymphocytes. The compounds inducing lymphocytic activation were shown to elute, mainly near the void volume by size-exclusion chromatography, using Bio-Gel P6 (1-6kDa). Treatment of the compounds with chymotrypsin, a digestive protease, did not affect the induced B lymphocyte activation. On the contrary, hydrolysis with an α-l-arabinofuranosidase, removing single terminally-linked arabinose residues, decreased the extent of B cell activation. The immunostimulatory activity of these compounds was also observed by in vitro experiments, using bone marrow-derived macrophages and dendritic cells as responders. Altogether, these results show the relevance of single arabinose residues, present at the non-reducing end of polymeric compounds, to the coffee stimulatory activity in cells mediating innate and acquired immunity.

Instant coffee as a source of antioxidant-rich and sugar-free coloured compounds for use in bakery: Application in biscuits.

Ammonia caramels are the most common antioxidant colour agent used in bakery formulations, although their high sugars content. An alternative could be coffee melanoidins, which are brown coloured compounds with antioxidant properties, readily available from instant coffee. However, high caffeine content is limiting its direct application. To evaluate the possibility of obtaining coloured melanoidin-rich, sugars- and caffeine-poor fractions from instant coffee, in this work, simple procedures based on their ethanol insolubility (fraction EtPp) or retention by ultrafiltration (fraction HWSn) were exploited. Melanoidins incorporation into biscuits formulation (amounts of 1, 5 and 10% w/w related to flour content) resulted in acceptable coloured products with higher antioxidant activity. The biscuits supplemented with 1% EtPp or HWSn had a low caffeine content. The caffeine of one espresso coffee was equivalent to 130 biscuits containing EtPp and 31 biscuits containing HWSn. Besides, both fractions did not promote extra formation of acrylamide or 5-hydroxymethylfurfural during baking.