Bioactives from agricultural food by-products: application in food and health

2015 - 2016Agriculture and agri-food industry produce a large amount of residues in non-edible portions from cultivation and processing of crops. These wastes, considered by-products, give serious environment damage, if not properly disposed, also because of their seasonal production. Until a few years ago the only goal was the disposal of these by-products. Recently the researchers discovered the characteristics of these wastes and their possible exploitation as sources of interesting compounds and energy for pharmaceutical, cosmetics and nutraceutical sectors. Fruit and vegetable by-products, in fact, are rich in bioactive compounds, such as carotenoids, dietary fibers, minerals and phenolic compounds, with correlated beneficial health effects. In this context the activity of the PhD project evaluated agricultural by-products as sources of bioactive compounds. The aims of the present PhD project were the development of innovative and selective analytical methodologies, for determination of bioactive compounds, using liquid chromatography methods (UHPLC) coupled to UV-Vis spectroscopy and mass spectrometry (high resolution, HRMS and tandem mass, MS/MS), the improvement of new extraction techniques, which can optimize extraction yields, minimize costs and environmental impact, such as pressurized hot water extraction (PHWE), ultrasound assisted extraction (UAE) and supercritical antisolvent fractionation (SAF), and finally the study of antioxidant activity of obtained extracts, using chemical and biological assays (DPPH, ABTS, ORAC, CAA). The analysis of bioactive compounds in plant extracts through advanced sample preparation techniques and modern separation tools allows a comprehensive study of the matrix. The project, very relevant, was to provide innovative methodologies, procedures and final products for different companies of healthcare area, in terms of innovation, costs and profits. The project was divided into three major areas, corresponding to the three selected by-products. The determination of chemical profile and the development and optimization of innovative and green extraction procedure for recovery of bioactive compounds have been carried out for each matrix. Selected by-products were: the main artichoke by-products, bracts and leaves, derived from cultivation and industrial processing, hazelnut by-products, roasted skins, derived from kernel industrial processing, and aromatic plants by-products, distillation waste waters, derived from essential oils production. All by-products studied have proved to be low cost sources of bioactive compounds with antioxidant activity. Furthermore, among innovative extraction techniques, PHWE procedures have allowed obtaining final extracts selectively rich in compounds of interest without formation of artefacts, and compared to existing extraction methods were simple, fast, environmentally friendly and fully automated. Moreover my PhD project provided new analytical methods to standardize vegetable extracts. The most relevant results showed that discarded raw materials are suitable ingredients for the production of formulated health products and nutraceuticals. [edited by author]XV n.s. (XXIX

Green non-conventional techniques for the extraction of polyphenols from agricultural food by-products: A review

Food processing industry is accompanied with the generation of a great production of wastes and by-products exceptionally rich in bioactive compounds (especially phenolics), with antioxidant activity. The recovery of these health molecules constitutes a key point for the valorization of by-products, with the possibility of creating new ingredients to be used for the formulation of food and cosmetic products. One of the main limitations to reuse by-products is linked to the high cost to obtain bioactive compounds, consequently in order to exploit these resources commercially valuable it is necessary to develop inno-vative, economic and environmentally friendly extraction strategies. These extraction methods should be able to reduce petroleum solvents, energy consumption and chemical wastes, protecting both environ -ment and consumers and ensuring safe and high-quality final products. The purpose of this review is to summarize current knowledge and applications of the new extraction techniques such as supercritical fluid extraction, pressurized liquid extraction, ultrasound assisted extraction applied to polyphenols ex-traction from agricultural food by-products. Particular attention has been paid to theoretical background, highlighting mechanisms and safety precautions. Authors concluded that relevant results of these tech-niques represent an opportunity to industrial scale-up, improving the extraction yields, minimizing time, costs and environmental impact. (c) 2021 Elsevier B.V. All rights reserved

Development and Validation of a Method for the Determination of (E)-Resveratrol and Related Phenolic Compounds in Beverages Using Molecularly Imprinted Solid Phase Extraction

A molecularly imprinted polymer was prepared using (E)-resveratrol as template and was evaluated for multicomponent multiclass analysis of polyphenolic compounds in complex matrices such as natural and alcoholic beverages. Chromatographic evaluation of the polymer exhibited high selectivity for (E)-resveratrol and its structural analogues, quercetin, and other flavonoids. An analytical procedure based on molecularly imprinted solid phase extraction (MISPE) and high-performance liquid chromatography coupled to UV detector was developed and validated for determination of (E)-resveratrol and quercetin in wine and fruit juice samples. The specific binding capacity of the MIP was estimated as 80 μg g(-1) polymer by the cartridge test. MISPE sample pretreatment allows an excellent sample cleanup, enormously decreasing the number of coextracted potentially interfering compounds. Under the described conditions, by extracting 2 mL samples a clean extract is obtained and (E)-resveratrol and quercetin could be easily identified at concentration levels of, respectively, 1.5 and 7.0 μg L(-1)

Rapid and automated on-line solid phase extraction HPLCâ\u80\u93MS/MS with peak focusing for the determination of ochratoxin A in wine samples

This study reports a fast and automated analytical procedure based on an on-line SPE-HPLCâ\u80\u93MS/MS method for the automatic pre-concentration, clean up and sensitive determination of OTA in wine. The amount of OTA contained in 100 μL of sample (pH â\u89\u85 5.5) was retained and concentrated on an Oasis MAX SPE cartridge. After a washing step to remove matrix interferents, the analyte was eluted in back-flush mode and the eluent from the SPE column was diluted through a mixing Tee, using an aqueous solution before the chromatographic separation achieved on a monolithic column. The developed method has been validated according to EU regulation N. 519/2014 and applied for the analysis of 41 red and 17 white wines. The developed method features minimal sample handling, low solvent consumption, high sample throughput, low analysis cost and provides an accurate and highly selective results

Rapid and automated analysis of aflatoxin M1 in milk and dairy products by online solid phase extraction coupled to ultra-high-pressure-liquid-chromatography tandem mass spectrometry

This study reports a fast and automated analytical procedure for the analysis of aflatoxin M1 (AFM1) in milk and dairy products. The method is based on the simultaneous protein precipitation and AFM1 extraction, by salt-induced liquid-liquid extraction (SI-LLE), followed by an online solid-phase extraction (online SPE) coupled to ultra-high-pressure-liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) analysis to the automatic pre-concentration, clean up and sensitive and selective determination of AFM1. The main parameters affecting the extraction efficiency and accuracy of the analytical method were studied in detail. In the optimal conditions, acetonitrile and NaCl were used as extraction/denaturant solvent and salting-out agent in SI-LLE, respectively. After centrifugation, the organic phase (acetonitrile) was diluted with water (1:9 v/v) and purified (1. mL) by online C18 cartridge coupled with an UHPLC column. Finally, selected reaction monitoring (SRM) acquisition mode was applied to the detection of AFM1.Validation studies were carried out on different dairy products (whole and skimmed cow milk, yogurt, goat milk, and powder infant formula), providing method quantification limits about 25 times lower than AFM1 maximum levels permitted by EU regulation 1881/2006 in milk and dairy products for direct human consumption. Recoveries (86-102%) and repeatability (RSD < 3, n=. 6) meet the performance criteria required by EU regulation N. 401/2006 for the determination of the levels of mycotoxins in foodstuffs. Moreover, no matrix effects were observed in the different milk and dairy products studied.The proposed method improves the performance of AFM1 analysis in milk samples as AFM1 determination is performed with a degree of accuracy higher than the conventional methods. Other advantages are the reduction of sample preparation procedure, time and cost of the analysis, enabling high sample throughput that meet the current concerns of food safety and the public health protection

Pressurized hot water extraction of bioactive compounds from artichoke by-products

Artichoke by-products are a suitable source of health-promoting ingredients for the production of dietary supplements and food additives. A pressurized hot water extraction (PHWE) was developed to recover caffeoylquinic acids (CQAs) and flavone glycosides (FLs) from agro-industrial artichoke by-products. The main factors influencing PHWE efficiency and CQA isomerization (temperature, numbers of cycles, modifier, and extraction time) were carefully studied and optimized by response surface design. The proposed PHWE procedure provides an exhaustive extraction of CQAs and FLs (recoveries: 93–105% and 90–105%) from artichoke external bracts and leaves of different cultivars (p > 0.05), without significant formation of artefacts generated by high temperatures. PHWE extracts showed CQA and FL levels (14–37 mg/g and 3–19 mg/g, respectively) comparable to commercial products and marked antioxidative effects (EC5011–83 μg/mL) by cellular antioxidant activity assay in human hepatocarcinoma HepG2 cells. These results proved that PHWE is an excellent green technique to recover bioactive compounds from artichoke agro-industrial residues

Chemical profile and cellular antioxidant activity of artichoke by-products

Artichoke by-products, produced from agricultural procedures and the processing industry, represent a huge amount of discarded material. In this research, the main artichoke by-products, bracts and leaves, were characterized in terms of their bioactive constituents (phenolic compounds and inulin) and cellular antioxidant potential to estimate their nutraceutical potential. The ultrahigh-performance-ultraviolet detection-high resolution mass spectroscopy (UHPLC-UV-HRMS) profiles of both by-products show that 5-caffeoylquinic acid and 1,5-dicaffeoylquinic acid are the most abundant bioactive compounds, and the content of flavone glycosides can be used to discriminate between bracts and leaves. Artichoke by-products contain a remarkable overall phenolic content (0.5–1.7 g per 100 g dry matter), whereas they differ widely in the amounts of inulin with higher levels in bracts (3.8–8.2 g per 100 g dry matter). The cellular antioxidant activities of bract and leaf extracts (half maximal effective concentration (EC50) = 26.6–124.1 mg L−1) are better than or similar to that of a commercial leaf extract, and are related to the dicaffeoylquinic acid levels, particularly to 1,5-dicaffeoylquinic acid. These results reveal that artichoke by-products are a promising and cheap source of bioactive compounds. Bracts could be used as a source of inulin and caffeoylquinic acids for the production of food additives and nutraceuticals and also as an alternative to the traditional application of leaf extracts

Determination of phenolic compounds in honey using dispersive liquid–liquid microextraction

Honey is a valuable functional food rich in phenolic compounds with a broad spectrum of biological activities. Analysis of the phenolic compounds in honey is a very promising tool for the quality control, the authentication and characterization of botanical origin, and the nutraceutical research. This work describes a novel approach for the rapid analysis of five phenolic acids and 10 flavonoids in honey. Phenolic compounds were rapidly extracted and concentrated from diluted honey by dispersive liquid–liquid microextraction (DLLME) and then analyzed using high performance liquid chromatography with UV absorbance detection (HPLC–UV). Some important parameters, such as the nature and volume of extraction and dispersive solvents, pH and salt effect were carefully investigated and optimized to achieve the best extraction efficiency. Under the optimal conditions, an exhaustive extraction for twelve of the investigated analytes (recoveries >70%), with a precision (RSD < 10%) highly acceptable for complex matrices, and detection and quantification limits at ppb levels (1.4–12 and 4.7–40 ng g−1, respectively) were attained. The proposed method, compared with the most widely used method in the analysis of phenolic compounds in honey, provided similar or higher extraction efficiency, except in the case of the most hydrophilic phenolic acids. The capability of DLLME to the extraction of other honey phytochemicals, such as abscisic acid, was also demonstrated. The main advantages of developed method are the simplicity of operation, the rapidity to achieve a very high sample throughput and low cos

Clinical Impact of Enteral Protein Nutritional Therapy on Patients with Obesity Scheduled for Bariatric Surgery: A Focus on Safety, Efficacy, and Pathophysiological Changes

Background: Ketogenic diet-induced weight loss before bariatric surgery (BS) has beneficial effects on the reduction in the liver volume, metabolic profile, and intra- and post-operative complications. However, these beneficial effects can be limited by poor dietary adherence. A potential solution in patients showing a poor adherence in following the prescribed diet could be represented by enteral nutrition strategies. To date, no studies describe the protocol to use for the efficacy and the safety of pre-operative enteral ketogenic nutrition-based dietary protocols in terms of weight reduction, metabolic efficacy, and safety in patients with obesity scheduled for BS. Aims and scope: To assess the clinical impact, efficacy, and safety of ketogenic nutrition enteral protein (NEP) vs. nutritional enteral hypocaloric (NEI) protocols on patients with obesity candidate to BS. Patients and methods: 31 NEP were compared to 29 NEI patients through a 1:1 randomization. The body weight (BW), body mass index (BMI), waist circumference (WC), hip circumference (HC), and neck circumference (NC) were assessed at the baseline and at the 4-week follow-up. Furthermore, clinical parameters were assessed by blood tests, and patients were asked daily to report any side effects, using a self-administered questionnaire. Results: Compared to the baseline, the BW, BMI, WC, HC, and NC were significantly reduced in both groups studied (p &lt; 0.001). However, we did not find any significative difference between the NEP and NEI groups in terms of weight loss (p = 0.559), BMI (p= 0.383), WC (p = 0.779), and HC (p = 0.559), while a statistically significant difference was found in terms of the NC (NEP, -7.1% vs. NEI, -4%, p = 0.011). Furthermore, we found a significant amelioration of the general clinical status in both groups. However, a statistically significant difference was found in terms of glycemia (NEP, -16% vs. NEI, -8.5%, p &lt; 0.001), insulin (NEP, -49.6% vs. NEI, -17.8%, p &lt; 0.0028), HOMA index (NEP, -57.7% vs. NEI, -24.9%, p &lt; 0.001), total cholesterol (NEP, -24.3% vs. NEI, -2.8%, p &lt; 0.001), low-density lipoprotein (NEP, -30.9% vs. NEI, 1.96%, p &lt; 0.001), apolipoprotein A1 (NEP, -24.2% vs. NEI, -7%, p &lt; 0.001), and apolipoprotein B (NEP, -23.1% vs. NEI, -2.3%, p &lt; 0.001), whereas we did not find any significative difference between the NEP and NEI groups in terms of aortomesenteric fat thickness (p = 0.332), triglyceride levels (p = 0.534), degree of steatosis (p = 0.616), and left hepatic lobe volume (p = 0.264). Furthermore, the NEP and NEI treatments were well tolerated, and no major side effects were registered. Conclusions: Enteral feeding is an effective and safe treatment before BS, with NEP leading to better clinical results than NEI on the glycemic and lipid profiles. Further and larger randomized clinical trials are needed to confirm these preliminary data

Selective extraction of high-value phenolic compounds from distillation wastewater of basil (Ocimum basilicum L.) by pressurized liquid extraction

During the essential oil steam distillation from aromatic herbs, huge amounts of distillation wastewaters (DWWs) are generated. These by-products represent an exceptionally rich source of phenolic compounds such as rosmarinic acid (RA) and caffeic acid (CA). Herein, the alternative use of dried basil DWWs (dDWWs) to perform a selective extraction of RA and CA by pressurized liquid extraction (PLE) employing bio-based solvent was studied. To select the most suitable solvent for PLE, the theoretical modelling of Hansen solubility parameters (HSP) was carried out. This approach allows reducing the list of candidate to two solvents: ethanol and ethyl lactate. Due to the composition of the sample, mixtures of water with those solvents were also tested. An enriched PLE extract in RA (23.90 ± 2.06 mg/g extract) with an extraction efficiency of 75.89 ± 16.03% employing a water-ethanol mixture 25:75 (% v/v) at 50°C was obtained. In the case of CA, a PLE extract with 2.42 ± 0.04 mg/g extract, having an extraction efficiency of 13.86 ± 4.96% using ethanol absolute at 50°C was achieved. DWWs are proposed as new promising sources of natural additives and/or functional ingredients for cosmetic, nutraceutical, and food applications