Papers by Marcello Locatelli
Pomegranate fruit is a functional food of high interest for human health due to its wide range of... more Pomegranate fruit is a functional food of high interest for human health due to its wide range of phytochemicals with antioxidant properties are implicated in the prevention of inflammation and cancer. Ellagitannins, such as punicalagin and ellagic acid, play a role as anti-atherogenic and neuroprotective molecules in the complex fighting against the degenerative diseases. The aim of this work was to evaluate the composition in punicalagins and ellagic acid of differently obtained extracts from whole fruit, peels and juices, prepared by squeezing or by centrifugation, of pomegranate belonging to different cultivars. Moreover, a wider phenolic fingerprint was also determined. The bioactivity of the extracts was tested on the redox activity of PDIA3 disulfide isomerase, an enzyme involved in the regulation of several cellular functions and associated with different diseases such as cancer, prion disorders, Alzheimer’s and Parkinson’s diseases. The results demonstrate that the differen...
This study aims to establish the biological and chemical profile of Asphodeline liburnica (Scop.)... more This study aims to establish the biological and chemical profile of Asphodeline liburnica (Scop.) Rchb. root. The antioxidant, antimicrobial, enzyme inhibitory, DNA protection, apoptotic DNA ladder fragmentation analysis, and anti-proliferative of A. liburnica were established using standard assays. In silico study was also performed to understand interactions between quantified anthraquinones and key enzymes of clinical relevance. Total phenolic and flavonoid contents were found to be 9.67 mgGAE/g and 1.48 mgRE/g extract, respectively. Chrysophanol was detected as a major anthraquinone. The extract exhibited radical scavenging ability against DPPH and ABTS with values of 13.23 and 66.99 mgTE/g extract, respectively. Good inhibitory activity against tyrosinase was recorded. In silico experiments showed that the anthraquinones were able to establish coordinative bonds with the copper atoms present in the enzymatic cavity of tyrosinase. MTT cell viability test on MDA-MB-231 cells show...
A pro-drug is a substance administered in a pharmacologically inactive structure that, once admin... more A pro-drug is a substance administered in a pharmacologically inactive structure that, once administered, is metabolised in vivo into the corresponding active principle. The rationale for the design of prodrugs is the optimisation of absorption, distribution, metabolism, and excretion (ADME). Moreover these compounds are frequently synthesized to improve bioavailability. 5-Amino salicylic acid (5-ASA) represents one of the most efficient agents for ColoRectal Cancer (CRC) treatment. Its inclusion in natural or semi-synthetic cyclodextrins (CDs) has been extensively studied to enhance drug properties as solubility, stability, and bioavailability. On the other hand, very recently naturally occurring 4'- geranyloxyferulic acid and auraptene were found as novel promising agents for the treatment of colon diseases, like adenomas and adenocarcinomas. In this review we will focus our attention on the reported pharmacological activity and analytical assays for the most representative 5-...
Journal of Chromatography B
Molecules
Analysis of 4-cyanophenol and 3-nitrophenol was carried out using multi-walled carbon nanotubes-b... more Analysis of 4-cyanophenol and 3-nitrophenol was carried out using multi-walled carbon nanotubes-based solid-phase extraction (SPE) and capillary electrophoresis (CE) methods. Capillary electrophoresis was carried out with 18 kV voltage, 214 nm detection, and phosphate buffer (pH 7.0, 15 mM) as background electrolyte at 25 ± 1 °C temperature with 15.05 and 16.5 min migration times of 4-cyanophenol and 3-nitrophenol. The separation and resolution factors were 1.10 and 2.90. The optimized experimental conditions were 40 mg/L concentration, 1.0 g multi-walled carbon nanotubes (MWCNTs) per SPE cartridge, 5.0 mL/min flow rate of water, 0.1 mL flow rate of eluting solvent. The maximum recoveries were 91% and 98% at 0.1 mL/min flow rate of 4-cyanophenol and 3-nitrophenol. These methods were applied successfully for extraction and estimation of 4-cyanophenol and 3-nitrophenol in the municipal wastewater. The reported methods are reproducible, efficient, and practical for the estimation of th...
Phytochemical Analysis
INTRODUCTION The analysis of plant and herbal samples is a challenging task for analytical chemis... more INTRODUCTION The analysis of plant and herbal samples is a challenging task for analytical chemists due to the complexity of the matrix combined with the low concentration of analytes. In recent years different liquid-phase microextraction (LPME) techniques coupled with a variety of analytical equipment have been developed for the determination of both organic and inorganic analytes. OBJECTIVE Over the past few years, the number of research papers in this field has shown a markedly growing tendency. Therefore, the purpose of this review paper is to summarise and critically evaluate research articles focused on the application of LPME techniques for the analysis of plant and herbal samples. RESULTS Due to the complex nature of the samples, the direct application of LPME techniques to the analysis of plants has not often been done. LPME techniques as well as their modalities have been commonly applied in combination with other pretreatment techniques, including a solid-liquid extraction technique supported by mechanical agitation or auxiliary energies for plant analysis. Applications and the most important parameters are summarised in the tables. CONCLUSION This review summarises the application of the LPME procedure and shows the major benefits of LPME, such as the low volume of solvents used, high enrichment factor, simplicity of operation and wide selection of applicable detection techniques. We can expect further development of microextraction analytical methods that focus on direct sample analysis with the application of green extraction solvents while fully automating procedures for the analysis of plant materials.
Separations
Recently, high demand of high-throughput analyses with high sensitivity and selectivity to molecu... more Recently, high demand of high-throughput analyses with high sensitivity and selectivity to molecules and drugs in different classes with different physical-chemical properties—and a reduction in analysis time—is a principal milestone for novel methodologies that researchers are trying to achieve—especially when analytical procedures are applied to clinical purposes. In addition, to avoid high doses of a single drug that could cause serious side effects, multi-drug therapies are often used to treat numerous diseases. For these reasons, the demand for methods that allow the rapid analysis of mixed compounds has increased in recent years. In order to respond to these needs, new methods and instruments have been developed. However, often the complexity of a matrix can require a long time for the preparation and processing of the samples. Different problems in terms of components, types of matrices, compounds and physical-chemical complexity are encountered when considering drugs associa...
Analytica
Nowadays, the challenges in analytical chemistry, and mostly in quantitative analysis, include th... more Nowadays, the challenges in analytical chemistry, and mostly in quantitative analysis, include the development and validation of new materials, strategies and procedures to meet the growing need for rapid, sensitive, selective and green methods. In this context, considering the constantly updated International Guidelines, constant innovation is mandatory both in the pre-treatment procedures and in the instrumental configurations to obtain reliable, true, and reproducible information. In this context, additionally to the classic plasma (or serum) matrices, biopsies, whole blood, and urine have seen an increase in the works that also consider non-conventional matrices. Obviously, all these studies have shown that there is a correlation between the blood levels and those found in the new matrix, in order to be able to correlate and compare the results in a robust way and reduce any bias problems. This review provides an update of the most recent developments currently in use in the sam...
Pharmaceutics
Mesoporous silicon microparticles (MSMPs) can incorporate drug-carrying nanoparticles (NPs) into ... more Mesoporous silicon microparticles (MSMPs) can incorporate drug-carrying nanoparticles (NPs) into their pores. An NP-loaded MSMP is a multistage vector (MSV) that forms a Matryoshka-like structure that protects the therapeutic cargo from degradation and prevents its dilution in the circulation during delivery to tumor cells. We developed an MSV constituted by 1 µm discoidal MSMPs embedded with PEGylated liposomes containing oxaliplatin (oxa) which is a therapeutic agent for colorectal cancer (CRC). To obtain extra-small liposomes able to fit the 60 nm pores of MSMP, we tested several liposomal formulations, and identified two optimal compositions, with a prevalence of the rigid lipid 1,2-distearoyl-sn-glycero-3-phosphocholine and of 1,2-distearoyl-sn-glycero-3-phosphoethanolamine-N-[methoxy(polyethylene glycol)-2000]. To improve the MSV assembly, we optimized the liposome-loading inside the MSMP and achieved a five-fold increase of the payload using an innovative lyophilization appro...
Antioxidants
Even though Salvia genus is one of the most known and studied taxa of Lamiaceae family, the knowl... more Even though Salvia genus is one of the most known and studied taxa of Lamiaceae family, the knowledge regarding the chemical composition and health-related benefits of some locally used Salvia species (mostly endemic) is still scarce. In this regard, the present work aims to evaluate the chemical profile and potential bioactivities of 70% (v/v) ethanolic extracts obtained from the less-studied S. transsylvanica and S. glutinosa in comparison with S. officinalis. HPLC-PDA analysis revealed the presence of rutin and catechin as the main compounds in the extracts of the three studied species (using the employed HPLC method), whereas the presence of naringenin was highlighted only in S. glutinosa extract. Chlorogenic acid, rutin and quercetin were identified and quantified for the first time in S. transsylvanica extracts. The in vitro antioxidant capacity of each extract was tested through complementary methods (phosphomolybdenum assay, DPPH, ABTS, CUPRAC and FRAP assays), and correlate...
Antioxidants
Sweet pepper is a typical type of Capsicum annuum from Abruzzo region, recognized as a traditiona... more Sweet pepper is a typical type of Capsicum annuum from Abruzzo region, recognized as a traditional and local product, traditionally cultivated in the town of Altino (Abruzzo region, Italy). The aim of this study is to compare the sweet type of peppers from Altino with the hot pepper cultivated in the same area, in order to delineate their different phytochemical and biological profiles in vitro and in vivo. In this study, we elucidated their phytochemical composition, fatty acids composition and phenolic/flavonoid contents in extracts. Then antioxidant and enzyme inhibition assays were performed to evaluate their biological properties, together with in vitro cell assay and in vivo anti-inflammatory activity. Microwave (1000 mg/mL) extract of hot pepper showed the best inhibition value on in vitro cell growth assay; in fact, the number of survived cells was about 20% and 40% for microwave and Soxhlet extracts, respectively. In vivo anti-inflammatory assay revealed good activity for b...
Food Research International
Frontiers in Pharmacology
Sideritis, also named "ironwort," "mountain tea," or "shepherd's tea," is a genus of flowering pl... more Sideritis, also named "ironwort," "mountain tea," or "shepherd's tea," is a genus of flowering plants used as herbal medicine in traditional Mediterranean-area medicine systems, and these plants are generally consumed as a herbal tea. Its use as herbal tea and in traditional herbal medicine is quite popular. There are currently few studies on Sideritis perfoliata L., and only one reports the use of a liquid chromatography coupled to diode array detection and electrospray ionization tandem mass spectrometry (LC-DAD-ESI-MS n) profile and the content of phenolic compounds without considering a possible correlation with its biological activities. This paper aims to investigate the antioxidant activities by means of several different biological/biochemical assays (radical scavenging, reducing power, ferrous ion chelating, and total antioxidant by phosphomolybdenum and b-carotene bleaching methods) as well as analyze the enzyme inhibitory activities (against AChE (acetylcholinesterase), BChE (butyrylcholinesterase), tyrosinase, a-glucosidase, and a-amylase) as well as the total phenolics, flavonoids, and condensed tannins. The reported results on Sideritis perfoliata highlighted that methanol and water extracts generally showed higher radical scavenging and reducing power activities. A similar trend could be observed for phosphomolybdenum and ferrous ion chelating activities. Methanol extracts showed lower activity only for the b-carotene bleaching assay.
Molecules
A sensitive, rapid, reliable, and easily applicable method based on magnetic solid phase extracti... more A sensitive, rapid, reliable, and easily applicable method based on magnetic solid phase extraction (MSPE) combined with HPLC-PDA was developed for monitoring propoxur (PRO) and fenitrothion (FEN) pesticides in environmental water samples. The effect of major experimental variables on the extraction efficiency of both the pesticides was investigated and optimized systematically. For this purpose, a new magnetic material containing decanoic acid on the surface of particles was synthesized and characterized by XRD, FT-IR, SEM, EDX, and TGA analysis in detail. The simultaneous determination of pesticide molecules was carried out by using a Luna Omega C18 column, isocratic elution of acetonitrile (ACN): Water (70:30 v/v) with a flow rate of 1.2 mL min−1. After MSPE, the linear range for pesticide molecules (r2 > 0.9982) was obtained in the range of 5–800 and 10–800 ng mL−1, respectively. The limit of detections (LOD) are 1.43 and 4.71 ng mL−1 for PRO and FEN, respectively while RSDs ...
Molecules
In this work, the synthesis, characterization, and application of novel parabens imprinted polyme... more In this work, the synthesis, characterization, and application of novel parabens imprinted polymers as highly selective solid-phase extraction (SPE) sorbents have been reported. The imprinted polymers were created using sol–gel molecular imprinting process. All the seven parabens were considered herein in order to check the phase selectivity. By means of a validated HPLC-photodiode array detector (PDA) method all seven parabens were resolved in a single chromatographic run of 25 min. These SPE sorbents, in-house packed in SPE empty cartridges, were first characterized in terms of extraction capability, breakthrough volume, retention volume, hold-up volume, number of theoretical plates, and retention factor. Finally, the device was applied to a real urine sample to check the method feasibility on a very complex matrix. The new paraben imprinted SPE sorbents, not yet present in the literature, potentially encourage the development of novel molecularly imprinted polymers (MIPs) to enha...
Molecules
Background: Galium is a plant rich in iridoid glycosides, flavonoids, anthraquinones, and small a... more Background: Galium is a plant rich in iridoid glycosides, flavonoids, anthraquinones, and small amounts of essential oils and vitamin C. Recent works showed the antibacterial, antifungal, antiparasitic, and antioxidant activity of this plant genus. Methods: For the determination of the multicomponent phenolic pattern, liquid phase microextraction procedures were applied, combined with HPLC-PDA instrument configuration in five Galium species aerial parts (G. verum, G. album, G. rivale, G. pseudoaristatum, and G. purpureum). Dispersive Liquid–Liquid MicroExtraction (DLLME) with NaCl and NAtural Deep Eutectic Solvent (NADES) medium and Ultrasound-Assisted (UA)-DLLME with β-cyclodextrin medium were optimized. Results: The optimal DLLME conditions were found to be: 10 mg of the sample, 10% NaCl, 15% NADES or 1% β-cyclodextrin as extraction solvent—400 μL of ethyl acetate as dispersive solvent—300 μL of ethanol, vortex time—30 s, extraction time—1 min, centrifugation at 12000× g for 5 min...
Trends in Food Science & Technology
Abstract Background Phenolic compounds present multiple health benefits due to their various biol... more Abstract Background Phenolic compounds present multiple health benefits due to their various biological activities such as antioxidant and anti-inflammatory activities, while also serving as functional food ingredients as they can substitute preservatives through their antioxidant and antibacterial activities. Unfortunately, many of such compounds are not only within cytosolic spaces but are also bound within plant cellular walls. Many extraction methods to this day are not able to access such compounds and thus obtain maximum yield levels. Enzyme-assisted extraction methods are currently one of the few types of methods capable of achieving this outcome, while also implying mild reaction conditions, substrate specificity, industrial applicability and other numerous advantages. Scope and approach The following study aims to provide thorough insights regarding these extraction methods in the hope of further familiarizing readers with these innovative extraction methods as they are currently yet to earn wide usage. Thus, a review of current available data selected from studies observing enzyme-assisted extractions of polyphenols as well as studies concerning enzyme-assisted extractions combined with other innovative chemical substances and/or instrumentations (such as ionic liquids, ultrasounds, microwaves, etc.). Key findings and conclusions Given the presented information, enzyme-assisted extraction methods enabled increased polyphenolic compound accessibility, allowing nearly whole plant matrix exploitation, through easily manipulable process parameters. Despite these highly appreciated advantages and high feasibility, enzyme-assisted extraction methods were found to be scarcely industrially implemented as a result of their novelty. Scientific papers such as this review attempt to encourage their understanding and popularization.
Separations
Antibiotics are a common practice in veterinary medicine, mainly for therapeutic purposes. Sector... more Antibiotics are a common practice in veterinary medicine, mainly for therapeutic purposes. Sectors of application include livestock farming, aquacultures, and bee-keeping, where bacterial infections are frequent and can be economically damaging. However, antibiotics are usually administered in sub-therapeutic doses as prophylactic and growth promoting agents. Due to their excessive use, antibiotic residues can be present in foods of animal origin, which include meat, fish, milk, eggs, and honey, posing health risks to consumers. For this reason, authorities have set maximum residue limits (MRLs) of certain antibiotics in food matrices, while analytical methods for their determination have been developed. This work focuses on antibiotic extraction and determination, part of which was presented at the "1st Conference in Chemistry for Graduate, Postgraduate Students and PhD Candidates at the Aristotle University of Thessaloniki". Taking a step further, this paper is a review of the most recent sample preparation protocols applied for the extraction of sulfonamide antibiotics from food samples and their determination with high-performance liquid chromatography (HPLC), covering a five-year period.
Nutrients
Pomegranate fruit is a functional food of high interest for human health due to its wide range of... more Pomegranate fruit is a functional food of high interest for human health due to its wide range of phytochemicals with antioxidant properties are implicated in the prevention of inflammation and cancer. Ellagitannins, such as punicalagin and ellagic acid, play a role as anti-atherogenic and neuroprotective molecules in the complex fighting against the degenerative diseases. The aim of this work was to evaluate the composition in punicalagins and ellagic acid of differently obtained extracts from whole fruit, peels and juices, prepared by squeezing or by centrifugation, of pomegranate belonging to different cultivars. Moreover, a wider phenolic fingerprint was also determined. The bioactivity of the extracts was tested on the redox activity of PDIA3 disulfide isomerase, an enzyme involved in the regulation of several cellular functions and associated with different diseases such as cancer, prion disorders, Alzheimer’s and Parkinson’s diseases. The results demonstrate that the differen...
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Papers by Marcello Locatelli