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Study of Influential Parameters of the Caffeine Extraction From clean technologies Article Study of Influential Parameters of the Caffeine Extraction from Spent Coffee Grounds: From Brewing Coffee Method to the Waste Treatment Conditions Alexandre Vandeponseele, Micheline Draye , Christine Piot and Gregory Chatel * EDYTEM, University Savoie Mont Blanc, CNRS, F-73000 Chambéry, France; [email protected] (A.V.); [email protected] (M.D.); [email protected] (C.P.) * Correspondence: [email protected] Abstract: This article aims to study the interest of spent coffee grounds (SCG) valorization through caffeine recovery. In an original way, this study takes into account all the parameters such as (i) the brewing coffee methods (household, coffee shops, etc.); (ii) the storage conditions, in particular the drying step; (iii) the solid/liquid extraction parameters such as the nature of solvent, the temperature, the extraction time and the solid/liquid ratio; and (iv) the liquid/liquid purification parameters such as the nature, the volume and the pH of extraction medium. Results have shown that spent coffee grounds from coffee-shops obtained by percolation contain a higher amount of caffeine than spent coffee grounds from households obtained from spent pods or filters. A drying treatment is not required when extraction is performed under one week after the spent coffee grounds collection −1 with 96.4% of not degraded caffeine. Solid/liquid extraction performed with 25 mL.g SCG of Citation: Vandeponseele, A.; Draye, hydroalcoholic solvent (water/EtOH, v/v 60/40) at 60 ◦C during 15 min have given a caffeine yield M.; Piot, C.; Chatel, G. Study of −1 up to 4.67 mg.g SCG. When using ethyl acetate, 93.4% of the caffeine has been selectively recovered Influential Parameters of the Caffeine by liquid/liquid extraction. Finally, the extraction of caffeine for the valorization of spent coffee Extraction from Spent Coffee grounds is a promising and easy way, which fits with an already important and well established Grounds: From Brewing Coffee market. Method to the Waste Treatment Conditions. Clean Technol. 2021, 3, 335–350. https://doi.org/10.3390/ Keywords: spent coffee grounds; biomass valorization; caffeine; storage conditions; extraction cleantechnol3020019 parameters; purification Academic Editor: Patrick Cognet Received: 31 January 2021 1. Introduction Accepted: 3 March 2021 Coffee is one of the most being traded commodity with an annual world production Published: 2 April 2021 over 10 million tons in 2019 [1]. The path to produce a coffee beverage is long and leads to the generation of several by-products such as coffee husk, pulp, silverskin and spent Publisher’s Note: MDPI stays neutral coffee grounds (SCG). Coffee grounds represent the most valuable and available coffee with regard to jurisdictional claims in by-product produced by soluble coffees industries, domestic houses, restaurants and coffee published maps and institutional affil- shops. Besides, it has been calculated that 650 kg of spent coffee grounds are generated iations. from one ton of green coffee beans turned into coffee beverage [2]. Spent coffee grounds has been studied for high value applications such as production of biodiesel [3,4], bioethanol [5,6], biopolymer such as polyhydroxyalkanoate (PHA) [7,8], adsor- bent for air depollution [9] or water depollution [10], and extracts of bioactive molecules Copyright: © 2021 by the authors. such as polyphenols and caffeine [11–21]. Indeed, 1,3,7-trimethyl-1H-purine-2,6(3H,7H)- Licensee MDPI, Basel, Switzerland. dione, also called 1,3,7–trimethylxanthine or caffeine for coffee, theine for tea or guara- This article is an open access article nine for guarana, is the most widely used psychotropic substance all over the world distributed under the terms and (Figure1)[22]. conditions of the Creative Commons Caffeine can be incorporated in daily life products such as sodas and energy drinks [23], Attribution (CC BY) license (https:// painkillers [24] or slimming creams [25]. Nowadays, coffee decaffeination is the most im- creativecommons.org/licenses/by/ portant known process to recover caffeine [26,27]. Extracted caffeine is the same as synthetic 4.0/). Clean Technol. 2021, 3, 335–350. https://doi.org/10.3390/cleantechnol3020019 https://www.mdpi.com/journal/cleantechnol Clean Technol. 2021, 3 336 Clean Technol. 2021, 3, FOR PEER REVIEWcaffeine, expect that its economic value is higher due to its naturalness. However, caffeine2 from spent coffee grounds is rarely purified from raw extracts of bioactive molecules [18]. FigureFigure 1.1. TheThe chemicalchemical structurestructure ofof 1,3,7–trimethylxanthine1,3,7–trimethylxanthine (caffeine).(caffeine). Hence,Caffeine the can aim be of incorporated this work is toin proposedaily life a products full investigation such as ofsodas parameters and energy of caffeine drinks production[23], painkillers from [24] spent or slimming coffee grounds creams such [25]. as: Nowadays, (i) the brewing coffee decaffeination method in relation is the withmost theimportant origin of known spent process coffee grounds to recover (household, caffeine [26, restaurants/coffee27]. Extracted caffeine shops), is the (ii) same the storage as syn- conditionsthetic caffeine, with expect the influence that its of economic a drying value step, (iii)is higher the first due step to ofits solid/liquidnaturalness. extractionHowever, tocaffeine recover from caffeine spent from coffee spent grounds coffee is groundsrarely pu (naturerified from of the raw solvent, extracts extraction of bioactive tempera- mole- turecules and [18]. time, solid/liquid ratio) and (iv) the second step of liquid/liquid extraction to selectivelyHence, recover the aim caffeine of this work (nature is to and propose volume a offull the investigation solvent, pH). of parameters of caffeine production from spent coffee grounds such as: (i) the brewing method in relation with the 2.origin Materials of spent and coffee Methods grounds (household, restaurants/coffee shops), (ii) the storage con- 2.1.ditions Chemicals with the and influence Reagents of a drying step, (iii) the first step of solid/liquid extraction to recoverPure caffeine standard from of spent caffeine, coffee ethanol grounds (96% (nat purity,ure of notthe denatured),solvent, extraction acetic temperature acid (99.5% purity)and time, and solid/liquid dichloromethane ratio) wereand (iv) obtained the second from ACROSstep of liquid/liquid ORGANICS. extraction Acetonitrile, to ethylselec- acetate,tively recovern-heptane caffeine and sodium(nature hydroxideand volume were of the supplied solvent, by pH). Fisher Chemical. Chlorhydric acid (37% w) was obtained from Roth. All solvents and reagents were of analytical grade and2. Materials used as received.and Methods 2.1. Chemicals and Reagents 2.2. Plant Material Pure standard of caffeine, ethanol (96% purity, not denatured), acetic acid (99.5% pu- Spent coffee grounds and roasted coffee beans used in this study have been obtained fromrity) aand local dichloromethane bakery (R1) and were from obtained two restaurants from ACROS (R2, R3). ORGANICS. The bakery Acetonitrile, and restaurants ethyl prepareacetate, coffeen-heptane beverage and sodium using the hydroxide brewing were method supplied called by percolation Fisher Chemical. using professional Chlorhydric high-pressureacid (37% w) was coffeemakers. obtained fromThe roastedRoth. All coffee solvents beans and are reagents from the were same of provider analytical for grade each restaurantand used as and received. are composed of a blend of 80% of Arabica and 20% of Robusta coffee. Indi- viduals obtain spent coffee grounds through different ways: by percolation with household capsule2.2. Plant coffeemakers Material (C1, C2), by percolation with mocha coffeemaker (M1) and by filtration with filterSpent coffeemakers coffee grounds (F1). andThe roasted amount coffee of water beans required used in to this brew study the coffeehave been was differentobtained forfrom the a householdlocal bakery capsule (R1) and coffeemakers from two restau C1, C2rants (13 mL/g(R2, R3).coffee The), household bakery and filtration restaurants cof- feemakerprepare coffee F1 (18 beverage mL/gcoffee using), mocha the brewing coffeemaker method M1 called (unknown percolation ratio) and using restaurants professional R1, R2,high-pressure R3 (unknown coffeemakers. ratio). The The residence roasted time coffee of waterbeans are inside from coffee the same were provider unknown for in each all cases.restaurant and are composed of a blend of 80% of Arabica and 20% of Robusta coffee. Individuals obtain spent coffee grounds through different ways: by percolation with 2.3.household Storage ofcapsule Spent Coffeecoffeemakers Grounds (C1, (SCG) C2), by percolation with mocha coffeemaker (M1) and Theby filtration spent coffee with grounds filter coffeemakers from the bakery (F1). (R1)The wereamount used of for water the studyrequired ofstorage to brew and the solid/liquidcoffee was different extraction. for the A full household week was capsule required coffeemakers for the bakery C1, C2 to (13 fill mL/g up a 25coffee L), plastichouse- buckethold filtration with spent coffeemaker coffee grounds F1 (18 mL/g that wascoffee), then mocha closed. coffeemaker The naturally M1 (unknown wet (59.25% ratio) water and w/wrestaurants) spent coffeeR1, R2, grounds R3 (unknown were then ratio). stored The atresidence standard time pressure of water and inside temperature coffee were in a ◦ closeunknown plastic in bucket.all cases. Dry spent coffee grounds were
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