PMID- 34885901 OWN - NLM STAT- MEDLINE DCOM- 20220208 LR - 20220208 IS - 1420-3049 (Electronic) IS - 1420-3049 (Linking) VI - 26 IP - 23 DP - 2021 Dec 2 TI - Microwave-Assisted Extraction of Phenolic Compounds from Spent Coffee Grounds. Process Optimization Applying Design of Experiments. LID - 10.3390/molecules26237320 [doi] LID - 7320 AB - In this study, sustainable technology microwave-assisted extraction (MAE) in association with green solvents was applied to recover phenolic compounds from spent coffee grounds (SCGs). A design of experiments (DOE) was used for process optimization. Initially, a 2(4-1) two level Fractional Factorial Design was used and ratios "solvent to solute" and "ethanol to water" were identified as the significant experimental factors. Consequently, Central Composite Design (CCD) was applied to analyze the effects of the significant variables on the response yield, total polyphenols content (TPC), and antioxidant activity (AA) by the DPPH assay method, and quadratic surfaces to optimize those responses were generated. The values of the significant factors of 16.7 (solvent/solute) and 68.9% (ethanol/water) were optimized simultaneously the yield (%) at 6.98 +/- 0.27, TPC (mg GAE/g) at 117.7 +/- 6.1, and AA (micromol TE/g) at 143.8 +/- 8.6 and were in excellent agreement with those predicted from the CCD model. The variations of the compositions of the lipids, caffeine, pentacyclic diterpenes, and FAME as a function of the dominant factor % ethanol in the solvent mixture were analyzed by applying NMR and GC-FID, and the results obtained confirmed their determinative significance. FAU - Coelho, Jose P AU - Coelho JP AUID- ORCID: 0000-0001-8118-0864 AD - Instituto Superior de Engenharia de Lisboa, Instituto Politecnico de Lisboa, Rua Conselheiro Emidio Navarro 1, 1959-007 Lisboa, Portugal. AD - Centro de Quimica Estrutural, Instituto Superior Tecnico, Universidade de Lisboa, Av. Rovisco Pais 1, 1049-001 Lisboa, Portugal. FAU - Robalo, Maria P AU - Robalo MP AUID- ORCID: 0000-0002-8200-6910 AD - Instituto Superior de Engenharia de Lisboa, Instituto Politecnico de Lisboa, Rua Conselheiro Emidio Navarro 1, 1959-007 Lisboa, Portugal. AD - Centro de Quimica Estrutural, Instituto Superior Tecnico, Universidade de Lisboa, Av. Rovisco Pais 1, 1049-001 Lisboa, Portugal. FAU - Boyadzhieva, Stanislava AU - Boyadzhieva S AD - Institute of Chemical Engineering, Bulgarian Academy of Sciences, Academic Georgi Bontchev str., 1113 Sofia, Bulgaria. FAU - Stateva, Roumiana P AU - Stateva RP AUID- ORCID: 0000-0002-4834-8183 AD - Institute of Chemical Engineering, Bulgarian Academy of Sciences, Academic Georgi Bontchev str., 1113 Sofia, Bulgaria. LA - eng GR - UIDB/00100/2020/Fundacao para a Ciencia e Tecnologia/ GR - 778168/European Union's Horizon 2020, Marie Sklodow-Curie/ GR - DH 07/12/Ministry of Education and Science of Bulgaria/ PT - Journal Article DEP - 20211202 PL - Switzerland TA - Molecules JT - Molecules (Basel, Switzerland) JID - 100964009 RN - 0 (Phenols) RN - 0 (Plant Extracts) RN - 0 (Solvents) SB - IM MH - Coffea/*chemistry MH - Microwaves MH - Phenols/analysis/*isolation & purification MH - Plant Extracts/analysis/*isolation & purification MH - Seeds/chemistry MH - Solvents PMC - PMC8658841 OTO - NOTNLM OT - design of experiments OT - green technology OT - microwave extraction OT - spent coffee grounds OT - total polyphenols content COIS- The authors declare no conflict of interest. The funders had no role in the design of the study; in the collection, analyses, or interpretation of the data; in the writing of the manuscript; or in the decision to publish the results. EDAT- 2021/12/11 06:00 MHDA- 2022/02/09 06:00 PMCR- 2021/12/02 CRDT- 2021/12/10 01:08 PHST- 2021/10/28 00:00 [received] PHST- 2021/11/28 00:00 [revised] PHST- 2021/11/30 00:00 [accepted] PHST- 2021/12/10 01:08 [entrez] PHST- 2021/12/11 06:00 [pubmed] PHST- 2022/02/09 06:00 [medline] PHST- 2021/12/02 00:00 [pmc-release] AID - molecules26237320 [pii] AID - molecules-26-07320 [pii] AID - 10.3390/molecules26237320 [doi] PST - epublish SO - Molecules. 2021 Dec 2;26(23):7320. doi: 10.3390/molecules26237320.