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Abstract The degradation in water of furosemide (FUR), a widely used diuretic drug, was herein reported. The method entails an integrated approach based on the hybridisation of hydrodynamic cavitation (HC) with electrical discharge (ED) plasma technology. This dynamic duo could increase the production of oxidising compounds in water, in particular hydroxyl radicals (OH radicals), by triggering the rapid homolytic decomposition of water molecules and avoiding the addition of external oxidants. This study clearly emphasises the effectiveness of an integrated approach to improve the degradation of pollutants in wastewater originating from active pharmaceutical ingredients (APIs). The results of HC/ED-assisted FUR degradation in the presence of radical scavengers highlight the predominant role of the radical oxidation mechanism at the gas–liquid interface of the cavitation bubble during HC/ED treatment. A comparative analysis of the three technologies—HC alone, HC/ED and UV alone—emphasised the promising potential of hybrid HC/ED as a scalable industrial technology. This is demonstrated by the higher degradation rates (100%, 10 min) when treating large volumes (5L) of wastewater contaminated with FUR (50 mg/L), even in the presence of other APIs.

The industrial preparation of kudzu starch (KS) significantly reduces the remaining of flavonoids like puerarin (PU) in the product, weakening its biological activity and making pre-treatments on kudzu crucial. Ultrasonic technique, widely used for modifying biomolecules, can enhance nutrient interactions like those between starch and polyphenols in foods. Thus, a puerarin-kudzu starch (PKS) complex was prepared with the introduction of ultrasonic pretreatment. The results indicated that sonication increased the binding of PU to KS from 0.399 ± 0.01 to 0.609 ± 0.05 mg/g. Particle size analysis and SEM revealed that the particles of the ultrasonic puerarin-kudzu starch complex (UPKS) were larger than those of the untreated complexes. XRD, UV–vis, and FT-IR spectroscopic analyses indicated that hydrogen bonding primarily governs the interaction between PU and KS. Additionally, incorporating PU decreased the starch structure’s orderliness, while ultrasonic treatment altered the helical configuration of straight-chain starch, leading to the formation of a new, ordered structure through the creation of new hydrogen bonds. Additionally, gels formed from UPKS exhibited higher viscosity, elasticity, and shear stress, suggesting that ultrasound significantly altered the intermolecular interactions between PKS. In conclusion, the use of ultrasound under optimal conditions has demonstrated its effectiveness in preparing PKS complexes, highlighting its significant potential to produce high value-added kudzu-based products.

With the aim of developing a sustainable and efficient extraction of polyphenols-rich fraction from Sorbus spp., Microwave-Assisted Subcritical Water Extraction (MASWE) was selected as the technique of choice. Although Sorbus spp. berries are rich in nutraceutical compounds, they are generally underutilised. The extracts obtained contain caffeoylquinic acids (i.e. chlorogenic acids), flavonoids, and organic acids, all of which are active components with potential applications in innovative functional foods due to their potent antioxidant activity. To optimise the extraction protocol, different temperatures and different species of the above genus were studied to improve the recovery of the polyphenolic fractions and obtain products with potential high bioactivity. The best resulting sample was studied more in detail using different colorimetric assays (total content of polyphenols, flavonoids and sugars – TPC, 406.43 mgGAE/gext; TFC, 13.5 mgQE/gext; TSC, 454.1 mgGlu/gext), purification streams, and LC-MS analyses. However, the most remarkable property observed is the outstanding antioxidant activity of the extract (4.74 mmolTrolox.eq/gext). In order to obtain a refined product rich in bioactive compounds, a purification protocol was performed leading to a final TPC selectivity of about 87 % and 10.12 mmolTrolox.eq/gext. Qualitative LC-MS analyses helped to identify chlorogenic acids as predominant in the extract, along with methyl esters of sorbic acid.

The extraction of bioactive compounds from food by-products is one of the most important research areas for the nutraceutical, pharmaceutical, and food industries. This research aimed to evaluate the efficiency of Ultrasound-Assisted Extraction (UAE) and Microwave-Assisted Extraction (MAE), either alone or in combination, of phenolic compounds from cocoa bean shells (CBSs). These extraction techniques were compared with conventional methods, such as under simple magnetic stirring and the Soxhlet apparatus. After the preliminary characterization of the gross composition of CBSs, the total polyphenol content and radical scavenging of extracts obtained from both raw and defatted cocoa bean shells were investigated. Quantification of the main polyphenolic compounds was then performed by RP-HPLC-DAD, identifying flavonoids and phenolic acids, as well as clovamide. The application of MAE and UAE resulted in a similar or superior extraction of polyphenols when compared with traditional methods; the concentration of individual polyphenols was variously influenced by the extraction methods employed. Combining MAE and UAE at 90 °C yielded the highest antiradical activity of the extract. Spectrophotometric analysis confirmed the presence of high-molecular-weight melanoidins, which were present in higher concentrations in the extracts obtained using MAE and UAE, especially starting from raw material. In conclusion, these results emphasize the efficiency of MAE and UAE techniques in obtaining polyphenol-rich extracts from CBS and confirm this cocoa by-product as a valuable biomass for the recovery of antioxidant compounds, with a view to possible industrial scale-up.

Extra virgin olive oil (EVOO) is a cornerstone of the Mediterranean diet. Many studies have highlighted its crucial preventive role against cardiovascular disease, neurodegenerative disorders, metabolic syndrome and cancer, with these effects being due to the synergistic anti-inflammatory and antioxidant activities of minor components, such as polyphenols and tocols. The aim of the present study is to implement new technologies for olive oil mills and develop an efficient large-sized industrial process for the continuous extraction of healthier EVOOs that are enriched with these bioactive compounds. Non-thermal technologies, namely ultrasound (US) and pulsed electric field (PEF), have been tested, separately and in combination, to eliminate the need for traditional malaxation. There is extensive literature to support the efficacy of ultrasound-assisted extraction (UAE) and PEF treatments in EVOO production. A newly designed US device and a PEF industrial chamber have been combined into a single, integrated continuous-flow setup, the performance of which in the extraction of EVOO from green Coratina olives has been evaluated herein. Extraction yields, physico-chemical and organoleptic characteristics, and polyphenol and tocol contents were monitored throughout the trials, and the last three were measured at accelerated aging times (AAT) of 15 and 30 days. The US and combined US-PEF processes not only increased daily oil production (ton/day, by nearly 45%), but also eliminated the need for kneading during malaxation, resulting in significant energy savings (approximately 35%). In addition, these innovations enriched the resulting EVOO with nutritionally relevant minor components (8–12% polyphenols, 3–5% tocols), thereby elevating its quality and market value, as well as overall stability. The introduction of continuous-flow US and PEF technologies is a remarkable innovation for the EVOO industry, as they offer benefits to both producers and consumers. The EVOO resulting from non-thermal continuous-flow production meets the growing demand for healthier, nutrient-enriched products.

Nowadays, the world is facing a general problem of resource overconsumption and waste overproduction: to address these two issues, the United Nations delivered the 12th Sustainable Development Goal (SDG), which has the objective of ensuring sustainable consumption and production patterns. Currently, polymers are present in every aspect of our lives and have the disadvantage of mostly coming from fossil sources and causing pollution when disposed of the wrong way. Agriculture plays a key role in the overall world environmental issues, being responsible for the creation of between 13 and 21% of global greenhouse gas (GHG) emissions. Moreover, it represents a continuously growing field, producing large amounts of waste. These residues can cause serious environmental concerns and high costs when disposed. However, agri-food waste (AFW) is a natural source of natural biopolymers, such as lignin, cellulose, pectin, and starch, but can also be used as a substrate to produce other non-toxic and biodegradable biopolymers, such as chitosan, polyhydroxyalkanoates (PHAs), and polylactic acid (PLA) through microbial fermentation. These polymers find applications in agricultural practices such as mulching films, soil stabilizers, hydrogels, nanocarriers, and coating for seeds, fruits, and vegetables. The employment of AFW in the production of non-toxic, sustainable, and biodegradable biopolymers for their agricultural utilization is an example of a virtuous circular economy approach that could help agriculture to be more sustainable.

In this paper, complexes of soluble dietary fiber (SDF) and polyphenols (PPs) isolated from lotus roots were prepared (SDF-PPs), as well as physical mixtures (SDF&PPs), which were given to high-fat-diet (HFD)-fed mice. The results demonstrated that SDF-PPs improve lipid levels and reverse liver injury in hyperlipidemic mice. Western blotting and real-time quantitative Polymerase Chain Reaction (RT-qPCR) results showed that SDF-PPs regulated liver lipids by increasing the phosphorylation of Adenine monophosphate activated protein kinase (AMPK), up-regulating the expression of Carnitine palmitoyltransferase1 (CPT1), and down-regulating the expression of Fatty acid synthase (FAS) and 3-hydroxy-3-methyl glutaryl coenzyme A (HMG-CoA), as well as the transcription factor sterol-regulatory element binding protein (SPEBP-1) and its downstream liposynthesis genes. Additionally, the intervention of SDF-PPs could modulate the composition of intestinal gut microbes, inducing an increase in Lachnospiraceae and a decrease in Desulfovibrionaceae and Prevotellaceae in high-fat-diet-fed mice. Thus, the research provides a theoretical basis for the application of lotus root active ingredients in functional foods and ingredients.

The United Nations Environment Programme’s (UNEP’s) Food Waste Index Report 2021 highlights a global annual food waste of 1 billion tons. The UNEP plays a crucial role in achieving Sustainable Development Goal (SDG) 12.3, which aims to halve per capita global food waste (FW) at the retail and consumer levels and reduce food losses along production and supply chains globally by 2030. On the other hand, the agricultural sector faces the challenge of increasing productivity to feed the world’s growing population while reducing the environmental impact on ecosystems and human health. In this context, the conversion of agri-food waste (AFW) into biocides, bio-based fertilizers (BBFs) and biostimulants could represent a successful approach to tackle all these issues. This review shows the latest findings on the different sources of AFW and the application of their bioactive compounds in agriculture. Increasing crop yields and improving plant physiology through the utilization of AFW-derived value products aligns with a circular economy approach, bolstering people’s confidence in managing food waste for improved food production.

Antibiotics (ABX) residues frequently occurred in water and cow milk. This work aims to understand the kinetics and mechanisms of sonolytic degradation of four ABX, i.e. ceftiofur hydrochloride (CEF), sulfamonomethoxine sodium (SMM), marbofloxacin (MAR), and oxytetracycline (OTC) in water and milk. In both water and milk, the sonolytic degradation of ABX follows pseudo-first order (PFO) kinetics well (R2: 0.951–0.999), with significantly faster ABX degradation in water (PFO kinetics constants (k1): 1.5 × 10−3-1.2 × 10−1 min−1) than in milk (k1: 3.5 × 10−4-5.6 × 10−2 min−1). The k1 values for SMM degradation in water increased by 118% with ultrasonic frequency (40–120 kHz), 174% with ultrasonic frequency (80–500 kHz), 649% with ultrasonic power (73–259 W), 22% with bulk temperature (12–40℃), and by 68% with reaction volume (50–250 mL), respectively, in other things being equal. The relevant k1 values in milk increased by 326%, 231%, 122%, 10% as well as 82% with the above same effective factors, respectively. The oxidation by free radicals generated in situ dominates ABX degradation, and the hydrophobic CEF (54.0–971.7 nM min−1) and SMM (39.2–798.4 nM min−1) underwent faster degradation than the hydrophilic MAR (33.9–751.9 nM min−1) and OTC (33.8–545.3 nM min−1) in both water and milk. Adding an extra 0.5 mM H2O2 accelerated SMM degradation by 19% in water and 33% in milk. After 130–150 min sonication of 100 mL of 2.0 mg L−1 (6.62 μM) SMM in various milk with 500 kHz and 259 W, the residue concentrations (52.9–96.3 μg L−1) can meet the relevant maximum residue limit (100 μg L−1).

The 2nd International Electronic Conference on Processes: Process Engineering—Current State and Future Trends (ECP 2023) was hosted online from 17 to 31 May 2023 [...]

The development of selective extraction protocols for Cannabis-inflorescence constituents is still a significant challenge. The characteristic Cannabis fragrance can be mainly ascribed to monoterpenes, sesquiterpenes and oxygenated terpenoids. This work investigates the entrapment of Cannabis terpenes in olive oil from inflorescences via stripping under mild vacuum during the rapid microwave-assisted decarboxylation of cannabinoids (MW, 120 °C, 30 min) and after subsequent extraction of cannabinoids (60 and 100 °C). The profiles of the volatiles collected in the oil samples before and after the extraction step were evaluated using static headspace solid-phase microextraction (HS-SPME), followed by gas chromatography coupled to mass spectrometry (GC-MS). Between the three fractions obtained, the first shows the highest volatile content (~37,400 mg/kg oil), with α-pinene, β-pinene, β-myrcene, limonene and trans-β-caryophyllene as the main components. The MW-assisted extraction at 60 and 100 °C of inflorescences using the collected oil fractions allowed an increase of 70% and 86% of total terpene content, respectively. Considering the initial terpene amount of 91,324.7 ± 2774.4 mg/kg dry inflorescences, the percentage of recovery after decarboxylation was close to 58% (mainly monoterpenes), while it reached nearly 100% (including sesquiterpenes) after extraction. The selective and efficient extraction of volatile compounds, while avoiding direct contact between the matrix and extraction solvents, paves the way for specific applications in various aromatic plants. In this context, aromatized extracts can be employed to create innovative Cannabis-based products within the hemp processing industry, as well as in perfumery, cosmetics, dietary supplements, food, and the pharmaceutical industry.

Mechanochemical treatment of various organic molecules is an emerging technology of green processes in biofuel, fine chemicals, or food production. Many biopolymers are involved in isolating, derivating, or modifying molecules of natural origin. Mechanochemistry provides a powerful tool to achieve these goals, but the unintentional modification of biopolymers by mechanochemical manipulation is not always obvious or even detectable. Although modeling molecular changes caused by mechanical stresses in cavitation and grinding processes is feasible in small model compounds, simulation of extrusion processes primarily relies on phenomenological approaches that allow only tool- and material-specific conclusions. The development of analytical and computational techniques allows for the inline and real-time control of parameters in various mechanochemical processes. Using artificial intelligence to analyze process parameters and product characteristics can significantly improve production optimization. We aim to review the processes and consequences of possible chemical, physicochemical, and structural changes.

Textiles and nonwovens (including those used in ventilation systems as filters) are currently one of the main sources of patient cross-infection. Healthcare-associated infections (HAIs) affect 5–10% of patients and stand as the tenth leading cause of death. Therefore, the development of new methods for creating functional nanostructured coatings with antibacterial and antiviral properties on the surfaces of textiles and nonwoven materials is crucial for modern medicine. Antimicrobial filter technology must be high-speed, low-energy and safe if its commercialization and mass adoption are to be successful. Cerium oxide nanoparticles can act as active components in these coatings due to their high antibacterial activity and low toxicity. This paper focuses on the elaboration of a high-throughput and resource-saving method for the deposition of cerium oxide nanoparticles onto nonwoven fibrous material for use in air-conditioning filters. The proposed spraying technique is based on the use of an aerodynamic emitter and simultaneous suction. Cerium oxide nanoparticles have successfully been deposited onto the filter materials used in air conditioning systems; the antibacterial activity of the ceria-modified filters exceeded 4.0.

In this study, a novel hydrodynamic cavitation unit combined with a glow plasma discharge system (HC-GPD) was proposed for the degradation of pharmaceutical compounds in drinking water. Metronidazole (MNZ), a commonly used broad-spectrum antibiotic, was selected to demonstrate the potential of the proposed system. Cavitation bubbles generated by hydrodynamic cavitation (HC) can provide a pathway for charge conduction during glow plasma discharge (GPD). The synergistic effect between HC and GPD promotes the production of hydroxyl radicals, emission of UV light, and shock waves for MNZ degradation. Sonochemical dosimetry provided information on the enhanced formation of hydroxyl radicals during glow plasma discharge compared to hydrodynamic cavitation alone. Experimental results showed a MNZ degradation of 14% in 15 min for the HC alone (solution initially containing 300 × 10−6 mol L−1 MNZ). In experiments with the HC-GPD system, MNZ degradation of 90% in 15 min was detected. No significant differences were observed in MNZ degradation in acidic and alkaline solutions. MNZ degradation was also studied in the presence of inorganic anions. Experimental results showed that the system is suitable for the treatment of solutions with conductivity up to 1500 × 10−6 S cm−1. The results of sonochemical dosimetry showed the formation of oxidant species of 0.15 × 10−3 mol H2O2 L−1 in the HC system after 15 min. For the HC-GPD system, the concentration of oxidant species after 15 min reached 13 × 10−3 mol H2O2 L−1. Based on these results, the potential of combining HC and GPD systems for water treatment was demonstrated. The present work provided useful information on the synergistic effect between hydrodynamic cavitation and glow plasma discharge and their application for the degradation of antibiotics in drinking water.

In submitting conference proceedings to Engineering Proceedings, the volume editors of the proceedings certify to the publisher that all papers published in this volume have been subjected to peer review administered by the volume editors [...]

Pomegranate (Punica granatum L.) is well known for its high content of bioactives, including polyphenols, flavonoids, and tannins, which have been shown to exhibit a wide range of biological activities, such as antioxidant, antimicrobial, and anticancer effects. It is worth noting that the majority of these molecules are found in the peels, which are usually disposed of after processing, causing a significant amount of waste, amounting to more than 3.6 million t/y. This work investigates microwave-assisted extraction (MAE) in water for the recovery of antioxidants from pomegranate peels (PP), including the optimisation of temperature and extraction times. The total phenolic, anthocyanin, flavonoid, and tannin contents of the recovered extracts were determined, as well as their antioxidant activities, which were found to be 356.35 mgGAE/gExtr, 303.97 µgCy3G/gExtr, 37.28 mgQE/gExtr, 56.48 mgGAE/gExtr, and 5.72 mmolTE/gExtr, respectively (according to the adopted reference). All results were compared with those obtained using a conventional protocol. In addition, the potential for water recycling by means of downstream nanofiltration in optimised MAE was investigated, leading to overall water reuse of approx. 75%. Power consumption (20.92 W/mgGAE) and common green metrics, Reaction Mass Efficiency (RME), E-Factor, and the Process Mass Intensiti/efficiency (PMI, PME), were considered in evaluating the proposed PP valorisation strategy. Finally, the biological activities of the main products were assessed. The antimicrobial properties of the PP extracts against three Gram-positive and three Gram-negative bacteria and their antiproliferative activity towards human cancer cells were tested. S. aureus bacteria was the most susceptible to the PP extracts. All tested products displayed antiproliferative activity against HeLa cells when higher concentrations were tested, with D-PP/NF (obtained from dried PP and sequential nanofiltration) being the most effective. This result was also confirmed via clonogenic analysis, which generally indicated the possible anti-cancer activity of pomegranate peel extracts obtained using this green approach.

Spherical SiO2 nanoparticles (SSNs) have been inventively synthesized using the Stöber method with sonication at medium–high frequencies (80, 120, and 500 kHz), aiming to control SSN size and shorten reaction time. Compared to the conventional method, such sonication allowed the Stöber reaction complete in 20–60 min with a low molar ratio of NH4OH/tetraethyl orthosilicate (0.84). The hydrodynamic diameters of 63–117 nm of SSNs were obtained under sonication with 80, 120, and 500 kHz of ultrasonic frequencies. Moreover, the SSNs obtained were smaller at 120 kHz than at 80 kHz in a multi-frequencies ultrasonic reactor, and the SSN size decreased with increasing ultrasonic power at 20 °C, designating the sonochemical unique character, namely, the SSN-size control is associated with the number of microbubbles originated by sonication. With another 500 kHz ultrasonic bath, the optimal system temperature for producing smaller SSNs was proven to be 20 °C. Also, the SSN size decreased with increasing ultrasonic power. The smallest SSNs (63 nm, hydrodynamic diameter by QELS, or 21 nm by FESEM) were obtained by sonication at 207 W for 20 min at 20 °C. Furthermore, the SSN size increased slightly with increasing sonication time and volume, favoring the scale-up of SSNs preparation. The mechanisms of controlling the SSN size were further discussed by the radical’s role and effects of ammonia and ethanol concentration.

Industrial organic synthesis is time and energy consuming, and generates substantial waste. Traditional conductive heating and mixing in batch reactors is no longer competitive with continuous-flow synthetic methods and enabling technologies that can strongly promote reaction kinetics. These advances lead to faster and simplified downstream processes with easier workup, purification and process scale-up. In the current Industry 4.0 revolution, new advances that are based on cyber-physical systems and artificial intelligence will be able to optimize and invigorate synthetic processes by connecting cascade reactors with continuous in-line monitoring and even predict solutions in case of unforeseen events. Alternative energy sources, such as dielectric and ohmic heating, ultrasound, hydrodynamic cavitation, reactive extruders and plasma have revolutionized standard procedures. So-called hybrid or hyphenated techniques, where the combination of two different energy sources often generates synergistic effects, are also worthy of mention. Herein, we report our consolidated experience of all of these alternative techniques.

The recovery of valuable bioactive compounds from the main underutilised by-products of the food industry is one of the greatest challenges to be addressed in circular economy. Potato peels are the largest waste generated during potato processing. However, they could be a potential source of valuable bioactive compounds, such as polyphenols, that can be reused as natural antioxidants. Currently, environmentally benign enabling technologies and new types of non-toxic organic solvents for the extraction of bioactive compounds may dramatically improve the sustainability of these processes. This paper focuses on the potential inherent in the valorisation of violet potato peels (VPPs) by recovering antioxidants using natural deep eutectic solvents (NaDES) under ultrasound (US)- and microwave (MW)-assisted extraction. Both the enabling technologies provided performances that were superior to those of conventional extractions in terms of antioxidant activity determined by the DPPH· (2,2-diphenyl-1-picrylhydrazyl) assay. In particular, the most promising approach using NaDES is proven to be the acoustic cavitation with a Trolox eq. of 1874.0 mmolTE/gExtr (40 °C, 500 W, 30 min), vs. the 510.1 mmolTE/gExtr of hydroalcoholic extraction (80 °C, 4 h). The shelf-life of both hydroalcoholic and NaDES-VPPs extracts have been assessed over a period of 24 months, and found that NaDES granted a 5.6-fold shelf-life extension. Finally, the antiproliferative activity of both hydroalcoholic and NaDES-VPPs extracts was evaluated in vitro using the MTS assay on human tumour Caco-2 cells and normal human keratinocyte cells (HaCaT). In particular, NaDES-VPPs extracts exhibited a significantly more pronounced antiproliferative activity compared to the ethanolic extracts without a noteworthy difference between effects on the two cell lines.

Meropenem is currently the most common carbapenem in clinical applications. Industrially, the final synthetic step is characterized by a heterogeneous catalytic hydrogenation in batch mode with hydrogen and Pd/C. The required high-quality standard is very difficult to meet and specific conditions are required to remove both protecting groups [i.e., p-nitrobenzyl (pNB) and p-nitrobenzyloxycarbonyl (pNZ)] simultaneously. The three-phase gas–liquid–solid system makes this step difficult and unsafe. The introduction of new technologies for small-molecule synthesis in recent years has opened up new landscapes in process chemistry. In this context, we have investigated meropenem hydrogenolysis using microwave (MW)-assisted flow chemistry for use as a new technology with industrial prospects. The reaction parameters (catalyst amount, T, P, residence time, flow rate) in the move from the batch process to semi-continuous flow were investigated under mild conditions to determine their influence on the reaction rate. The optimization of the residence time (840 s) and the number of cycles (4) allowed us to develop a novel protocol that halves the reaction time compared to batch production (14 min vs. 30 min) while maintaining the same product quality. The increase in productivity using this semi-continuous flow technique compensates for the slightly lower yield (70% vs. 74%) obtained in batch mode.

The inflorescences of Humulus lupulus L. are the most valuable ingredient in the brewing industry. Only female cones are used as their bitterness and aroma, much associated with beer, are granted by the production of resins and essential oils, respectively. The traditional brewing process for the extraction of the organic volatiles in hops is called dry hopping. It consists of extended maceration at low temperature after the fermentation phase. New extraction technologies can improve extraction rates and product quality while saving time and money. This article proves that multiple-effect fractional condensation under a vacuum is suitable for flavouring applications and especially for performing dry hopping without contamination risks and reductions in hop amounts. This technique leads to the recovery of aqueous aromatic fractions that are very rich in hop sesquiterpenes and monoterpenes. These suspensions are extremely stable when stored at 5–8 °C and avoid degradation even after several months. This feature is crucial for the marketing of non-alcoholic beverages, where the dilution of essential oils is otherwise problematic.

The chestnut tree (Castanea sativa, Mill.) is a widespread plant in Europe whose fruits and wood has a relevant economic impact. Chestnut wood (CW) is rich in high-value compounds that exhibit various biological activities, such as antioxidant as well as anticarcinogenic and antimicrobial properties. These metabolites can be mainly divided into monomeric polyphenols and tannins. In this piece of work, we investigated a sustainable protocol to isolate enriched fractions of the above-mentioned compounds from CW residues. Specifically, a sequential extraction protocol, using subcritical water, was used as a pre-fractionation step, recovering approximately 88% of tannins and 40% of monomeric polyphenols in the first and second steps, respectively. The optimized protocol was also tested at pre-industrial levels, treating up to 13.5 kg CW and 160 L of solution with encouraging results. Ultra- and nanofiltrations were used to further enrich the recovered fractions, achieving more than 98% of the tannin content in the heavy fraction, whilst the removed permeate achieved up to 752.71 mg GAE/gext after the concentration (75.3%). Samples were characterized by means of total phenolic content (TPC), antioxidant activity (DPPH· and ABTS·), and tannin composition (hydrolysable and condensed). In addition, LC-MS-DAD was used for semiqualitative purposes to detect vescalagin/castalagin and vescalin/castalin, as well as gallic acid and ellagic acid. The developed valorization protocol allows the efficient fractionation and recovery of the major polyphenolic components of CW with a sustainable approach that also evaluates pre-industrial scaling-up.

Continuous-flow chemistry has become a mainstream process and a notable trend among emerging technologies for drug synthesis. It is routinely used in academic and industrial laboratories to generate a wide variety of molecules and building blocks. The advantages it provides, in terms of safety, speed, cost efficiency and small-equipment footprint compared to analog batch processes, have been known for some time. What has become even more important in recent years is its compliance with the quality objectives that are required by drug-development protocols that integrate inline analysis and purification tools. There can be no doubt that worldwide government agencies have strongly encouraged the study and implementation of this innovative, sustainable and environmentally friendly technology. In this brief review, we list and evaluate the development and applications of continuous-flow processes for antibiotic synthesis. This work spans the period of 2012–2022 and highlights the main cases in which either active ingredients or their intermediates were produced under continuous flow. We hope that this manuscript will provide an overview of the field and a starting point for a deeper understanding of the impact of flow chemistry on the broad panorama of antibiotic synthesis.

Many scientists are working hard to find green alternatives to classical synthetic methods. Today, state-of-the-art ultrasonic and grinding techniques already drive the production of organic compounds on an industrial scale. The physicochemical and chemical behavior of cyclodextrins often differs from the typical properties of classic organic compounds and carbohydrates. The usually poor solubility and complexing properties of cyclodextrins can require special techniques. By eliminating or reducing the amount of solvent needed, green alternatives can reform classical synthetic methods, making them attractive for environmentally friendly production and the circular economy. The lack of energy-intensive synthetic and purification steps could transform currently inefficient processes into feasible methods. Mechanochemical reaction mechanisms are generally different from normal solution-chemistry mechanisms. The absence of a solvent and the presence of very high local temperatures for microseconds facilitate the synthesis of cyclodextrin derivatives that are impossible or difficult to produce under classical solution-chemistry conditions. Although mechanochemistry does not provide a general solution to all problems, several good examples show that this new technology can open up efficient synthetic pathways.

Hexane is a solvent used extensively in the food industry for the extraction of various products such as vegetable oils, fats, flavours, fragrances, colour additives or other bioactive ingredients. As it is classified as a “processing aid”, it does not have to be declared on the label under current legislation. Therefore, although traces of hexane may be found in final products, especially in processed products, its presence is not known to consumers. However, hexane, and in particular the n-hexane isomer, has been shown to be neurotoxic to humans and has even been listed as a cause of occupational diseases in several European countries since the 1970s. In order to support the European strategy for a toxic-free environment (and toxic-free food), it seemed important to collect scientific information on this substance by reviewing the available literature. This review contains valuable information on the nature and origin of the solvent hexane, its applications in the food industry, its toxicological evaluation and possible alternatives for the extraction of natural products. Numerous publications have investigated the toxicity of hexane, and several studies have demonstrated the presence of its toxic metabolite 2,5-hexanedione (2,5-HD) in the urine of the general, non-occupationally exposed population. Surprisingly, a tolerable daily intake (TDI) has apparently never been established by any food safety authority. Since hexane residues are undoubtedly found in various foods, it seems more than necessary to clearly assess the risks associated with this hidden exposure. A clear indication on food packaging and better information on the toxicity of hexane could encourage the industry to switch towards one of the numerous other alternative extraction methods already developed.

The aim of the present study is to develop a new industrial process for the continuous-flow extraction of virgin olive oil (VOO) using the non-thermal ultrasound (US) and pulsed electric field (PEF) treatments. These technologies have been tested both separately and in combination, with the aim of making the malaxation step unnecessary. The ultrasound-assisted extraction (UAE) and PEF treatments are both effective technologies for VOO production and have been well documented in the literature. The present study combines a new continuous-flow set-up, with four US units and PEF treatment. The industrial-plant prototype is able to improve VOO yields, thanks to powerful non-thermal physical effects (acoustic cavitation and electroporation), from 16.3% up to 18.1%. Moreover, these technologies increased the content of nutritionally relevant minor components, which, in turn, improves VOO quality and its commercial value (overall tocopherols and tocotrienols improved from 271 mg/kg under the conventional process to 314 mg/kg under the US process). The combined UAE and US-PEF process also increased the extraction yield, while overcoming the need for kneading in the malaxation step and saving process water (up to 1512 L per working day). Continuous-flow US and PEF technologies may be a significant innovation for the VOO industry, with benefits both for oil millers and consumers. The VOO obtained via non-thermal continuous-flow production can satisfy the current trend towards healthier nutrient-enriched products.

The biologically-derived polymers polyhydroxyalkanoates (PHAs) are biodegradable and can be considered a valuable alternative to conventional fossil-based plastics. However, upstream and downstream processes for PHA production are characterized by high energy and chemical consumption and are not economically competitive with petroleum-based polymers. Aiming to improve both the environmental and economical sustainability of PHAs production, in this work, corn straw was used as raw material to obtain a mixture of fermentable sugars after microwave-assisted flash hydrolysis (2 min, 0.01 g/L, 50.7% yield). A mixed microbial culture enriched from dairy industry waste was used for fermentation in a shake flask, allowing us to achieve good poly(hydroxy-butyrate-co-hydroxy-valerate) yields (41.4%, after 72 h of fermentation). A scale-up in a stirred tank bioreactor (3 L) gave higher yields (76.3%, after 96 h), allowing in both cases to achieve a concentration of 0.42 g/L in the fermentation medium. The possibility of producing PHAs from agricultural waste using a mixed microbial culture from the food industry with enabling technologies could make the production of biopolymers more competitive.

Antibiotic residues in water are general health and environmental risks due to the antibiotic-resistance phenomenon. Sonication has been included among the advanced oxidation processes (AOPs) used to remove recalcitrant contaminants in aquatic environments. Sonochemical processes have shown substantial advantages, including cleanliness, safety, energy savings and either negligible or no secondary pollution. This review provides a wide overview of the different protocols and degradation mechanisms for antibiotics that either use sonication alone or in hybrid processes, such as sonication with catalysts, Fenton and Fenton-like processes, photolysis, ozonation, etc.

Ultrasound has been applied in food processing for various purpose, showing potential to advance the physical and chemical modification of natural compounds. In order to explore the effect of ultrasonic pretreatment on the complexation of inulin and tea polyphenols (TPP), different frequencies (25, 40, 80 kHz) and output power (40, 80, 120 W) were carried out. According to the comparison in particle size distribution and phenolic content of different inulin-TPP complexes, it was indicated that high-intensity ultrasonic (HIU) treatment (25 kHz, 40 W, 10 min) could accelerate the interaction of polysaccharides and polyphenols. Moreover, a series of spectral analysis including UV–Vis, FT-IR and NMR jointly evidenced the formation of hydrogen bond between saccharides and phenols. However, the primary structure of inulin and the polysaccharide skeleton were not altered by the combination. Referring to field emission scanning electron microscopy (FESEM), the morphology of ultrasound treated-complex presented a slight agglomeration in the form of bent sheets, compared to non-treated sample. The inulin-TPP complex also revealed better stability based on thermogravimetric analysis (TGA). Thus, it can be speculated from the identifications that proper ultrasonic treatment is promising to promote the complexation of some food components during processing.

This work presents a proof of concept for a green cyclodextrin derivatisation method that uses low-boiling epoxide reagents in a high-energy ball mill (HEBM). The simplified preparation and purification of low substitution-degree common (2-hydroxy)propylated β- and γ-cyclodextrins (β/γ-CDs) has been realised. The intelligent use of propylene oxide has also facilitated the more effective synthesis of highly substituted γ-CD. Epichlorohydrin-crosslinked CD-polymers (CDPs) have also been effectively prepared in the ball mill. The unoptimised preparations of soluble and insoluble CDPs displayed very small particle size distributions, while the prepared polymers currently have different complexation properties to those of their classically prepared analogues.

Full analytical data of Ecuadorian cocoa wastes (raw shells) and beans (as benchmark), are herein reported. A detailed characterization of production residues may pave the road to a zero-waste strategy for the cocoa industry. Multiple analytical techniques have been exploited to define the composition of the matrices, among them: elemental analyses, FTIR, Py-GC/MS/FID and UHPLC-ESI-MS/MS.Quali-quantitative data of carbohydrates, lipids, lignin, polyphenols, alkaloids and proteins have been obtained by Py-GC/MS/FID and UHPLC-ESI-MS/MS. Assignations are fully supported by literature references. The FAMEs composition of lipophilic UAE extract is also reported for sake of comparison with cocoa butter. This data collection completes a wider valorization work, “Cocoa bean shell waste valorisation; extraction from lab to pilot-scale cavitational reactors” (Grillo et al., 2018).

Cefonicid is a second-generation cephalosporin sold under the brand name Sintocef™. It is an injectable drug obtained via a freeze-drying process and is also available for oral preparations. The high-quality standard required is very challenging to satisfy, and current production protocols are characterized by steps that are lengthy and cumbersome, making the product unattractive for the international market. Industrial R&D is constantly working on the process optimization for API synthesis, with the aim of increasing productivity and decreasing production costs and waste. We herein report a new and efficient method for the synthesis of the cefonicid benzathine salt that provides a good yield and high product stability. The double-nucleophilic and lipophilic nature of N′,N″-dibenzylethylene diacetate enables the deformylation of the OH-protected group on the mandelic moiety and also enables product crystallization to occur. We demonstrate that the formyl group in the peculiar position has high reactivity, promoting an amidation reaction that deprotects a hydroxy group and generates a new C-N bond in the reaction by-product. Several amines and OH-protected groups have been studied, but none were able to replicate the excellent results of benzathine diacetate.

Valorization of agri-food residues to produce bio-based platform chemicals will enhance the transition to the bio-economy era. To this end, a sustainable process has been developed for the overall valorization of grape stalks (GS) according to a circular approach, starting from the lignin fraction to further deal with the cellulose-rich residue. This non-conventional protocol fully adheres to green chemistry principles, exploiting the so-called enabling technologies—mainly ultrasound and microwaves—for energy-saving innovative processes. Firstly, ultrasound-assisted extraction (UAE, 40 kHz, 200 W) demonstrated to be an excellent technique for GS delignification combined with natural deep eutectic solvents (NaDESs). Delignification enables isolation of the pertinent lignin framework and the potential to obtain a polyphenol-rich liquid fraction, focusing on the valorization of GS as source of bioactive compounds (BACs). Among the NaDESs employed, the combination of choline chloride (ChCl) and levulinic acid (LevA) (ChLevA) presented noteworthy results, enabling a delignification higher than 70%. LevA is one of the top-value biobased platform chemicals. In this work, a flash microwave (MW)-assisted process was subsequently applied to the cellulose-rich fraction remained after delignification, yielding 85% LevA. The regeneration of this starting compound to produce ChLevA can lead to a further biomass delignification cycle, thus developing a new cascade protocol for a full valorization of GS.

Lignin is a fascinating aromatic biopolymer with high valorization potentiality. Besides its extensive value in the biorefinery context, as a renewable source of aromatics lignin is currently under evaluation for its huge potential in biomedical applications. Besides the specific antioxidant and antimicrobial activities of lignin, that depend on its source and isolation procedure, remarkable progress has been made, over the last five years, in the isolation, functionalization and modification of lignin and lignin-derived compounds to use as carriers for biologically active substances. The aim of this review is to summarize the current state of the art in the field of lignin-based carrier systems, highlighting the most important results. Furthermore, the possibilities and constraints related to the physico–chemical properties of the lignin source will be reviewed herein as well as the modifications and processing required to make lignin suitable for the loading and release of active compounds.

Nowadays, the application of ultrasound (US) energy for assisting the lignocellulosic biomass and waste materials conversion into value-added products has dramatically increased. In this sense, this review covers theoretical aspects, promising applications, challenges and perspectives about US and its use for biomass treatment. The combination of US energy with a suitable reaction time, temperature and solvent contributes to the destruction of recalcitrant lignin structure, allowing the products to be used in thermochemical and biological process. The main mechanisms related to US propagation and impact on the fragmentation of lignocellulosic materials, selectivity, and yield of conversion treatments are discussed. Moreover, the synergistic effects between US and alternative green solvents with the perspective of industrial applications are investigated. The present survey analysed the last ten years of literature, studying challenges and perspectives of US application in biorefinery. We were aiming to highlight value-added products and some new areas of research.

Over the last two decades, the scientific community and industry have made huge efforts to develop environmental protection technologies. In particular, the scarcity of drinking water has prompted the investigation of several physico-chemical treatments, and synergistic effects have been observed in hyphenated techniques. Herein, we report the first example of water treatment under simultaneous hydrodynamic cavitation and plasma discharge with the intense generation of radicals, UV light, shock waves and charged particles. This highly reactive environment is well suited to the bulk treatment of polluted water (i.e. E. coli disinfection and organic pollutant degradation). We have developed a new prototype and have efficiently applied this hybrid technology to water disinfection and the complete degradation of methanol in water with the aim of demonstrating its scalability. We have analyzed the mechanisms of water disinfection under the abovementioned conditions and verified them by measuring cavitation noise spectra and plasma emission spectra. We have also used the degradation of textile dyes and methanol solutions as an indicator for the formation of radicals.

Chestnut peels are a poorly characterized, underexploited by-product of the agri-food industry. This raw material is rich in bioactive compounds, primarily polyphenols and tannins, that can be extracted using different green technologies. Scaling up the process for industrial production is a fundamental step for the valorization of the extract. In this study, subcritical water extraction was investigated to maximize the extraction yield and polyphenol content. Lab-scale procedures have been scaled up to the semi-industrial level as well as the downstream processes, namely, concentration and spray drying. The extract antioxidant capacity was tested using in vitro and cellular assays as well as a preliminary evaluation of its antiadipogenic activity. The temperature, extraction time, and water/solid ratio were optimized, and the extract obtained under these conditions displayed a strong antioxidant capacity both in in vitro and cellular tests. Encouraging data on the adipocyte model showed the influence of chestnut extracts on adipocyte maturation and the consequent potential antiadipogenic activity. Chestnut peel extracts characterized by strong antioxidant power and potential antiadipogenic activity were efficiently obtained by removing organic solvents. These results prompted further studies on fraction enrichment by ultra- and nanofiltration. The semi-industrial eco-friendly extraction process and downstream benefits reported here may open the door to production and commercialization.

Cocoa husk is considered a waste product after cocoa processing and creates environmental issues. These waste products are rich in polyphenols, methylxanthine, dietary fibers, and phytosterols, which can be extracted and utilized in various food and health products. Cocoa beans represent only 32–34% of fruit weight. Various extraction methods were implemented for the preparation of extracts and/or the recovery of bioactive compounds. Besides conventional extraction methods, various studies have been conducted using advanced extraction methods, including microwave-assisted extraction (MAE), ultrasonic-assisted extraction (UAE), subcritical water extraction (SWE), supercritical fluid extraction (SFE), and pressurized liquid extraction (PLE). To include cocoa husk waste products or extracts in different food products, various functional foods such as bakery products, jam, chocolate, beverage, and sausage were prepared. This review mainly focused on the composition and functional characteristics of cocoa husk waste products and their utilization in different food products. Moreover, recommendations were made for the complete utilization of these waste products and their involvement in the circular economy.

Microwaves (MW) are often the most efficient, in terms of heat exchange and conversion rate, of all the energy sources used to promote chemical reactions thanks to fast volumetric dielectric heating, and metal-catalyzed synthetic reactions under heterogeneous conditions are an eloquent example. We herein report a MW-assisted green protocol for the C-H arylation of thiophenes with substituted aryl halides. This sustainable protocol carried out in γ-valerolactone (GVL) is catalyzed by Pd nanoparticles embedded in cross-linked β-cyclodextrin. In view of the excellent results achieved with activated substrates, the one-pot synthesis of a 4(3H)-quinazolinone derivative has been accomplished. A pressure-resistant MW reactor, equipped with multiple gas inlets, was used for sequential (i) C-H arylation, (ii) reduction, and (iii) carbonylation in the presence of the same catalyst, but under different gas atmospheres. The robust heterogeneous Pd catalyst showed limited metal leaching in GVL, making this an efficient MW-assisted process with high atom economy.

The search for sustainable alternatives for use in chemical synthesis and catalysis has found an ally in non-conventional energy sources and widely available green solvents. The use of glycerol, an abundant natural solvent, as an excellent “sacrificial” hydrogen source for the copper-catalyzed microwave (MW)-promoted transfer hydrogenation of nitrobenzene to aniline has been investigated in this work. Copper nanoparticles (CuNPs) were prepared in glycerol and the efficacy of the glycerol layer in mediating the interaction between the metal active sites has been examined using HRTEM analyses. Its high polarity, low vapor pressure, long relaxation time, and high acoustic impedance mean that excellent results were also obtained when the reaction media was subjected to ultrasound (US) and MW irradiation. US has been shown to play an important role in the process via its ability to enhance CuNPs dispersion, favor mechanical depassivation and increase catalytic active surface area, while MW irradiation shortened the reaction time from some hours to a few minutes. These synergistic combinations promoted the exhaustive reduction of nitrobenzene to aniline and facilitated the scale-up of the protocol for its optimized use in industrial MW reactors.

In the past, the use of mechanochemical methods in organic synthesis was reported as somewhat of a curiosity. However, perceptions have changed over the last two decades, and this technology is now being appreciated as a greener and more efficient synthetic method. The qualified “offer” of ball mills that make use of different set-ups, materials, and dimensions has allowed this technology to mature. Nevertheless, the intrinsic batch nature of mechanochemical methods hinders industrial scale-ups. New studies have found, in reactive extrusion, a powerful technique with which to activate chemical reactions with mechanical forces in a continuous flow. This new environmentally friendly mechanochemical synthetic method may be able to miniaturize production plants with outstanding process intensifications by removing organic solvents and working in a flow mode. Compared to conventional processes, reactive extrusions display high simplicity, safety, and cleanliness, which can be exploited in a variety of applications. This paper presents perspective examples in the better-known areas of reactive extrusions, including oxidation reactions, polymer processing, and biomass conversion. This work should stimulate further developments, as it highlights the versatility of reactive extrusion and the huge potential of solid-phase flow chemistry.

Interest in essential oils has consistently increased in recent years. Essential oils have a large variety of applications in multiple fields, including in the food, cosmetics and pharmaceutical industries. The volatile fraction (VF) in hops (Humulus lupulus L.) fits within this domain as it is primarily used in the brewery industry for the aromatization of beer, and is responsible for the floral and fruity tones. This work aims to design an optimized extraction protocol of the VF from hops, using microwaves. Microwave-assisted hydrodistillation (MAHD) has been developed to reduce energy and time consumption in lab-scale reactors up to industrial-scale systems. Hops are principally available in three forms, according to a brewery’s applications: (i) fresh (FH); (ii) dried (DH) and (iii) pelletized (PH). In this work, all three forms have therefore been studied and the recovered volatiles characterized by means of GC-MS. The optimized lab-scale MAHD protocol gave the best extraction yield of 20.5 mLVF/kgdry matrix for FH. This value underwent a slight contraction when working at the highest matrix amount (3 kg), with 17.3 mLVF/kgdry matrix being achieved. Further tests were then performed in a pilot reactor that is able to process 30 kg of material. In this case, high yield increases were observed for PH and DH; quadruple and double the lab-scale yields, respectively. In addition, this industrial-scale system also provided marked energy savings, practically halving the absorbed kJ/mLVF.

Flexible materials, such as fabric, paper and plastic, with nanoscale particles that possess antimicrobial properties have a significant potential for the use in the healthcare sector and many other areas. The development of new antimicrobial coating formulations is an urgent topic, as such materials could reduce the risk of infection in hospitals and everyday life. To select the optimal composition, a comprehensive analysis that takes into account all the advantages and disadvantages in each specific case must be performed. In this study, we obtained an antimicrobial textile with a 100% suppression of E. coli on its surface. These CeO2 nanocoatings exhibit low toxicity, are easy to manufacture and have a high level of antimicrobial properties even at very low CeO2 concentrations. High-power ultrasonic treatment was used to coat the surface of cotton fabric with CeO2 nanoparticles.

The selective synthesis of active pharmaceutical molecules is a challenging issue, particularly when attempting to make the reactions even more sustainable. The present work focuses on the microwave-assisted hydrogenolysis of oxytetracycline to selectively produce α-doxycycline. Although the combination of microwave irradiation and a heterogeneous rhodium catalyst provided good conversions, the selective synthesis of active α-doxycycline was only achieved when an oxytetracycline-cyclodextrin complex was used as the starting material, giving the desired product at 34.0% yield in a one-step reaction under very mild conditions.

Bromelain is a mixture of proteolytic enzymes that is extracted primarily from pineapples. It is present in almost all the aerial parts of the plant—the peels, leaves, stems and fruit—although only the fruit and stems contain significant amounts. The market-demand for bromelain is quickly increasing, especially in the health sector as it can be used as a drug and/or nutraceutical. Although the complete molecular mechanism has not been fully identified, bromelain possesses several properties, including anti-inflammatory, anti-oedema, antithrombotic and fibrinolytic, mucolytic, anticancer and cicatrizing effects that have been evaluated in several clinical trials. However, one of the main limitations for the clinical use of this supplement is the varying composition of extracts, which leads to heterogeneity in results and, therefore, difficulty in making evidence-based prescriptions. In fact, different geographic locations, land and modes of cultivation, as well as extraction methods, can all give extracts with different activities, depending on the plant part used. Additionally, although novel extraction techniques have been developed to improve bromelain purification and extraction and give higher yields without loss in enzymatic activity, these methods are still expensive and challenging. This review will describe the state of the art in the main conventional and unconventional extraction and purification methods of bromelain and discuss the advantages and limitations of these strategies. Pharmacokinetic and pharmacodynamic profiles and the clinical applications that have arisen from randomized controlled clinical trials are also discussed. Finally, future perspectives for bromelain extracts will be presented.

Cyclodextrin (CD) derivatives are a challenge, mainly due to solubility problems. In many cases, the synthesis of CD derivatives requires high-boiling solvents, whereas the product isolation from the aqueous methods often requires energy-intensive processes. Complex formation faces similar challenges in that it involves interacting materials with conflicting properties. However, many authors also refer to the formation of non-covalent bonds, such as the formation of inclusion complexes or metal–organic networks, as reactions or synthesis, which makes it difficult to classify the technical papers. In many cases, the solubility of both the starting material and the product in the same solvent differs significantly. The sweetest point of mechanochemistry is the reduced demand or complete elimination of solvents from the synthesis. The lack of solvents can make syntheses more economical and greener. The limited molecular movements in solid-state allow the preparation of CD derivatives, which are difficult to produce under solvent reaction conditions. A mechanochemical reaction generally has a higher reagent utilization rate. When the reaction yields a good guest co-product, solvent-free conditions can be slower than in solution conditions. Regioselective syntheses of per-6-amino and alkylthio-CD derivatives or insoluble cyclodextrin polymers and nanosponges are good examples of what a greener technology can offer through solvent-free reaction conditions. In the case of thiolated CD derivatives, the absence of solvents results in significant suppression of the thiol group oxidation, too. The insoluble polymer synthesis is also more efficient when using the same molar ratio of the reagents as the solution reaction. Solid reactants not only reduce the chance of hydrolysis of multifunctional reactants or side reactions, but the spatial proximity of macrocycles also reduces the length of the spacing formed by the crosslinker. The structure of insoluble polymers of the mechanochemical reactions generally is more compact, with fewer and shorter hydrophilic arms than the products of the solution reactions.

The present work addresses the development of an eco-friendly and cost-efficient protocol for the oxidation of primary and secondary alcohols to the corresponding aldehydes and ketones by mechanical processing under air. Ball milling was shown to promote the quantitative conversion of a broad set of alcohols into carbonyl compounds with no trace of an over-oxidation to carboxylic acids. The mechanochemical reaction exhibited higher yields and rates than the classical, homogeneous, TEMPO-based oxidation.

The present work focuses on the mechanochemical preparation of industrially important β-cyclodextrin (CD) derivatives. Activated CDs have been reacted with nitrogen and sulfur nucleophiles using a planetary mill equipped with stainless steel, zirconia and glass milling tools of different sizes. It is shown that the milling frequency and the number as well as the size of the milling balls have an effect on the nucleophilic reaction.