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This review is a collection of recent applications of mass spectrometry studies for the characterization of phytocannabinoids in cannabis and hemp plant material and related products. The focus is mostly on recent applications using mass spectrometry as detector, in hyphenation to typical separation techniques (i.e., liquid chromatography or gas chromatography), but also with less common couplings or by simple direct analysis. The papers are described starting from the most common approach for targeted quantitative analysis, with applications using low-resolution mass spectrometry equipment, but also with the introduction of high-resolution mass analysers as the detectors. This reflects a common trend in this field, and introduces the most recent applications using high-resolution mass spectrometry for untargeted analysis. The different approaches used for untargeted analysis are then described, from simple retrospective analysis of compounds without pure standards, through untargeted metabolomics strategies, and suspect screening methods, which are the ones currently allowing to achieve the most detailed qualitative characterization of the entire phytocannabinoid composition, including minor compounds which are usually overlooked in targeted studies and in potency evaluation. These approaches also represent powerful strategies to answer questions on biological and pharmacological activity of cannabis, and provide a sound technology for improved classification of cannabis varieties. Finally, open challenges are discussed for future directions in the detailed study of complex phytocannabinoid mixtures.
Anna Laura Capriotti; Giuseppe Cannazza; Martina Catani; Chiara Cavaliere; Alberto Cavazzini; Andrea Cerrato; Cinzia Citti; Simona Felletti; Carmela Maria Montone; Susy Piovesana; Aldo Laganà. Recent applications of mass spectrometry for the characterization of cannabis and hemp phytocannabinoids: from targeted to untargeted analysis. Journal of Chromatography A 2021, 462492 .
AMA StyleAnna Laura Capriotti, Giuseppe Cannazza, Martina Catani, Chiara Cavaliere, Alberto Cavazzini, Andrea Cerrato, Cinzia Citti, Simona Felletti, Carmela Maria Montone, Susy Piovesana, Aldo Laganà. Recent applications of mass spectrometry for the characterization of cannabis and hemp phytocannabinoids: from targeted to untargeted analysis. Journal of Chromatography A. 2021; ():462492.
Chicago/Turabian StyleAnna Laura Capriotti; Giuseppe Cannazza; Martina Catani; Chiara Cavaliere; Alberto Cavazzini; Andrea Cerrato; Cinzia Citti; Simona Felletti; Carmela Maria Montone; Susy Piovesana; Aldo Laganà. 2021. "Recent applications of mass spectrometry for the characterization of cannabis and hemp phytocannabinoids: from targeted to untargeted analysis." Journal of Chromatography A , no. : 462492.
The paper describes the development of a targeted quantitative method for the analysis of policosanols in hemp inflorescence. Policosanols are long chain aliphatic alcohols, with carbon chains typically in the range 20–36, with interesting biological activities. These compounds are typically separated by gas chromatography and only a few methods employ liquid chromatography for policosanols. In both cases, methods always include the derivatization of policosanols. In this study, policosanols were separated by ultra-high performance liquid chromatography without any derivatization and detected using high resolution mass spectrometry by formation of lithiated adducts. The procedure was optimized and a quantitative method was validated for the most abundant policosanols (with C24, C26, C27, C28, and C30 chain lengths) in industrial hemp inflorescence extracts. The method was used for the quantitative analysis of policosanols in five hemp types. Hemp wax was found rich in these compounds, especially C26 and C28 policosanols, which may prove useful for revalorization of wax by-products. Finally, the acquired data were also used to expand the search to the untargeted qualitative analysis of policosanols using Compound Discoverer. The untargeted method allowed the annotation of underivatized policosanols up to C33.
Carmela Maria Montone; Sara Elsa Aita; Giuseppe Cannazza; Chiara Cavaliere; Andrea Cerrato; Cinzia Citti; Luigi Mondello; Susy Piovesana; Aldo Laganà; Anna Laura Capriotti. Targeted and untargeted characterization of underivatized policosanols in hemp inflorescence by liquid chromatography-high resolution mass spectrometry. Talanta 2021, 235, 122778 .
AMA StyleCarmela Maria Montone, Sara Elsa Aita, Giuseppe Cannazza, Chiara Cavaliere, Andrea Cerrato, Cinzia Citti, Luigi Mondello, Susy Piovesana, Aldo Laganà, Anna Laura Capriotti. Targeted and untargeted characterization of underivatized policosanols in hemp inflorescence by liquid chromatography-high resolution mass spectrometry. Talanta. 2021; 235 ():122778.
Chicago/Turabian StyleCarmela Maria Montone; Sara Elsa Aita; Giuseppe Cannazza; Chiara Cavaliere; Andrea Cerrato; Cinzia Citti; Luigi Mondello; Susy Piovesana; Aldo Laganà; Anna Laura Capriotti. 2021. "Targeted and untargeted characterization of underivatized policosanols in hemp inflorescence by liquid chromatography-high resolution mass spectrometry." Talanta 235, no. : 122778.
Hemp and cannabis industry is undergoing a renewed interest due to legalization of marijuana (a topic that all countries are discussing, especially in recent years) and the growing importance of therapeutic properties of cannabinoids. Together with an increment in the production of hemp and recreational cannabis, there has been an increasing demand for accurate potency testing of products (i.e. quantification of main cannabinoids present in the plant in terms of weight percentage) prior commercialization. This translates in an urgent need of reliable analytical methods to characterize cannabis and hemp samples. Cannabis and hemp preparations are commercialized under various forms (e.g., flowers, oils, candies or even baked goods) usually containing a large number of often very similar compounds making their separation very challenging. Strictly connected to this, another emerging topic concerns the need for the developing of large scale separation techniques for the purification of cannabinoids from complex matrices and for the preparation of analytical-grade standards (including the chiral ones). This paper reviews the most recent achievements in both these aspects. Cutting-edge applications and novel opportunities in potency testing by high performance liquid chromatography (HPLC) with UV detection (which is becoming the golden standard, according to several pharmacopeias, for this kind of measurements) are discussed. The focus has been given to the very important topic of enantio-discrimination of chiral cannabinoids, for which supercritical fluid chromatography (SFC) appears to be particularly suitable. The last part of the work covers the purification of cannabinoids through preparative chromatography. In this regard, particular attention has been given to the most innovative multi-column techniques allowing for the continuous purification of target molecules. The most recent advancements and future challenges in this field are discussed.
Simona Felletti; Chiara De Luca; Alessandro Buratti; Desiree Bozza; Andrea Cerrato; Anna Laura Capriotti; Aldo Laganà; Alberto Cavazzini; Martina Catani. Potency testing of cannabinoids by liquid and supercritical fluid chromatography: Where we are, what we need. Journal of Chromatography A 2021, 1651, 462304 .
AMA StyleSimona Felletti, Chiara De Luca, Alessandro Buratti, Desiree Bozza, Andrea Cerrato, Anna Laura Capriotti, Aldo Laganà, Alberto Cavazzini, Martina Catani. Potency testing of cannabinoids by liquid and supercritical fluid chromatography: Where we are, what we need. Journal of Chromatography A. 2021; 1651 ():462304.
Chicago/Turabian StyleSimona Felletti; Chiara De Luca; Alessandro Buratti; Desiree Bozza; Andrea Cerrato; Anna Laura Capriotti; Aldo Laganà; Alberto Cavazzini; Martina Catani. 2021. "Potency testing of cannabinoids by liquid and supercritical fluid chromatography: Where we are, what we need." Journal of Chromatography A 1651, no. : 462304.
Soybeans (Glycine max) are an excellent source of dietary proteins and peptides with potential biological activities, such as antihypertensive, anti-cholesterol, and antioxidant activity; moreover, they could prevent cancer. Also, soy contains all the essential amino acids for nutrition; therefore, it represents an alternative to animal proteins. The goal of this paper was the comprehensive characterization of medium-sized and short peptides (two to four amino acids) obtained from simulated gastrointestinal digestion. Two different analytical approaches were employed for peptide characterization, namely a common peptidomic analysis for medium-sized peptides and a suspect screening analysis for short peptides, employing an inclusion list of exact m/z values of all possible amino acid combinations. Moreover, fractionation by preparative reversed-phase liquid chromatography was employed to simplify the starting protein hydrolysate. Six fractions were collected and tested for antioxidative activity by an innovative antioxidant assay on human gastric adenocarcinoma AGS cell lines. The two most active fractions (2 and 3) were then characterized by a peptidomic approach and database search, as well as by a suspect screening approach, in order to identify potential antioxidant amino acid sequences. Some of the peptides identified in these two fractions have been already reported in the literature for their antioxidant activity.
Chiara Cavaliere; Angela Montone; Sara Aita; Rosanna Capparelli; Andrea Cerrato; Paola Cuomo; Aldo Laganà; Carmela Montone; Susy Piovesana; Anna Capriotti. Production and Characterization of Medium-Sized and Short Antioxidant Peptides from Soy Flour-Simulated Gastrointestinal Hydrolysate. Antioxidants 2021, 10, 734 .
AMA StyleChiara Cavaliere, Angela Montone, Sara Aita, Rosanna Capparelli, Andrea Cerrato, Paola Cuomo, Aldo Laganà, Carmela Montone, Susy Piovesana, Anna Capriotti. Production and Characterization of Medium-Sized and Short Antioxidant Peptides from Soy Flour-Simulated Gastrointestinal Hydrolysate. Antioxidants. 2021; 10 (5):734.
Chicago/Turabian StyleChiara Cavaliere; Angela Montone; Sara Aita; Rosanna Capparelli; Andrea Cerrato; Paola Cuomo; Aldo Laganà; Carmela Montone; Susy Piovesana; Anna Capriotti. 2021. "Production and Characterization of Medium-Sized and Short Antioxidant Peptides from Soy Flour-Simulated Gastrointestinal Hydrolysate." Antioxidants 10, no. 5: 734.
Wild neotropical blueberries, endemic of Central and South American areas, are promising yet still undisclosed sources of bioactive compounds. Most research studies have addressed wild and cultivated blueberries from Europe and North America, despite the extremely wide variety of wild neotropical species. In the present paper, for the first time, the phenolic composition of Disterigma alaternoides was investigated through ultra-high-performance liquid chromatography coupled to high-resolution mass-spectrometric analysis followed by accurate data analysis and compound validation with a dedicated structure-based workflow. D. alaternoides, which belongs to a closely related genus to that of the common blueberry, grows exclusively in the Andean regions over 2000 above sea level. Thanks to the dedicated analytical platform, 249 phenolic compounds were tentatively identified, including several anthocyanins, flavonoids, phenolic acids, and proanthocyanidins. Thenature and heterogeneity of identified phenolic compounds demonstrate once more the need for a more profound knowledge of such still uncharted matrices.
Sara Aita; Anna Capriotti; Chiara Cavaliere; Andrea Cerrato; Benedetta Giannelli Moneta; Carmela Montone; Susy Piovesana; Aldo Laganà. Andean Blueberry of the Genus Disterigma: A High-Resolution Mass Spectrometric Approach for the Comprehensive Characterization of Phenolic Compounds. Separations 2021, 8, 58 .
AMA StyleSara Aita, Anna Capriotti, Chiara Cavaliere, Andrea Cerrato, Benedetta Giannelli Moneta, Carmela Montone, Susy Piovesana, Aldo Laganà. Andean Blueberry of the Genus Disterigma: A High-Resolution Mass Spectrometric Approach for the Comprehensive Characterization of Phenolic Compounds. Separations. 2021; 8 (5):58.
Chicago/Turabian StyleSara Aita; Anna Capriotti; Chiara Cavaliere; Andrea Cerrato; Benedetta Giannelli Moneta; Carmela Montone; Susy Piovesana; Aldo Laganà. 2021. "Andean Blueberry of the Genus Disterigma: A High-Resolution Mass Spectrometric Approach for the Comprehensive Characterization of Phenolic Compounds." Separations 8, no. 5: 58.
Cannabis sativa is traditionally classified according to five chemotypes based on the concentration of the main phytocannabinoids tetrahydrocannabinol (THC), cannabidiol (CBD), and cannabigerol (CBG). However, cannabis chemovars and varieties very often present similar concentrations of such phytocannabinoids but different chemical profiles, which is unavoidably translated into different pharmacological effects when used for therapeutic purposes. For this reason, a more refined approach is needed for chemovar distinction, which is described in this study and named phytocannabinomics. The classification was achieved by a comprehensive characterization of the phytocannabinoid composition, by liquid chromatography coupled to high-resolution mass spectrometry untargeted metabolomics for the detection of over a hundred phytocannabinoids, and data analysis by chemometrics for chemovars differentiation. The method was developed on fifty cannabis varieties, grown under the same conditions, and was validated to discriminate between the standard chemotypes by partial least squares discriminant analysis. Then, the method was extended to consider the entire chemical variety of the cannabis accessions, by an unsupervised approach based on the principal component analysis. The latter approach clearly indicated several new subgroups within the traditional classifications, which arise from a unique composition of the minor phytocannabinoids. The existence of these subgroups, which were never described before, is of critical importance for evaluating the pharmacological effects of cannabis chemovars.
Andrea Cerrato; Cinzia Citti; Giuseppe Cannazza; Anna Laura Capriotti; Chiara Cavaliere; Giampaolo Grassi; Federico Marini; Carmela Maria Montone; Roberta Paris; Susy Piovesana; Aldo Laganà. Phytocannabinomics: Untargeted metabolomics as a tool for cannabis chemovar differentiation. Talanta 2021, 230, 122313 .
AMA StyleAndrea Cerrato, Cinzia Citti, Giuseppe Cannazza, Anna Laura Capriotti, Chiara Cavaliere, Giampaolo Grassi, Federico Marini, Carmela Maria Montone, Roberta Paris, Susy Piovesana, Aldo Laganà. Phytocannabinomics: Untargeted metabolomics as a tool for cannabis chemovar differentiation. Talanta. 2021; 230 ():122313.
Chicago/Turabian StyleAndrea Cerrato; Cinzia Citti; Giuseppe Cannazza; Anna Laura Capriotti; Chiara Cavaliere; Giampaolo Grassi; Federico Marini; Carmela Maria Montone; Roberta Paris; Susy Piovesana; Aldo Laganà. 2021. "Phytocannabinomics: Untargeted metabolomics as a tool for cannabis chemovar differentiation." Talanta 230, no. : 122313.
Prostate cancer, a leading cause of cancer-related deaths worldwide, principally occurs in over 50-year-old men. Nowadays there is urgency to discover biomarkers alternative to prostate-specific antigen, as it cannot discriminate patients with benign prostatic hyperplasia from clinically significant forms of prostatic cancer. In the present paper, 32 benign prostatic hyperplasia and 41 prostatic cancer urine samples were collected and analyzed. Polar and positively charged metabolites were therein investigated using an analytical platform comprising an up to 40-fold analyte enrichment step by graphitized carbon black solid-phase extraction, HILIC separation, and untargeted high-resolution mass spectrometry analysis. These classes of compounds are often neglected in common metabolomics experiments even though previous studies reported their significance in cancer biomarker discovery. The complex metabolomics big datasets, generated by the UHPLC-HRMS, were analyzed with the ROIMCR procedure, based on the selection of the MS regions of interest data and their analysis by the Multivariate Curve-Resolution Alternating Least Squares chemometrics method. This approach allowed the resolution and tentative identification of the metabolites differentially expressed by the two data sets. Among these, amino acids and carnitine derivatives were tentatively identified highlighting the importance of the proposed methodology for cancer biomarker research.
Andrea Cerrato; Carmen Bedia; Anna Laura Capriotti; Chiara Cavaliere; Vincenzo Gentile; Martina Maggi; Carmela Maria Montone; Susy Piovesana; Alessandro Sciarra; Roma Tauler; Aldo Laganà. Untargeted metabolomics of prostate cancer zwitterionic and positively charged compounds in urine. Analytica Chimica Acta 2021, 1158, 338381 .
AMA StyleAndrea Cerrato, Carmen Bedia, Anna Laura Capriotti, Chiara Cavaliere, Vincenzo Gentile, Martina Maggi, Carmela Maria Montone, Susy Piovesana, Alessandro Sciarra, Roma Tauler, Aldo Laganà. Untargeted metabolomics of prostate cancer zwitterionic and positively charged compounds in urine. Analytica Chimica Acta. 2021; 1158 ():338381.
Chicago/Turabian StyleAndrea Cerrato; Carmen Bedia; Anna Laura Capriotti; Chiara Cavaliere; Vincenzo Gentile; Martina Maggi; Carmela Maria Montone; Susy Piovesana; Alessandro Sciarra; Roma Tauler; Aldo Laganà. 2021. "Untargeted metabolomics of prostate cancer zwitterionic and positively charged compounds in urine." Analytica Chimica Acta 1158, no. : 338381.
Industrial hemp (Cannabis sativa L.) represents an important plant, used for a variety of uses including pharmaceutical and nutraceutical purposes. As such, a detailed characterization of the composition of this plant could help future research to further exploit the beneficial effects of hemp compounds on the human health. Among the many compounds of hemp, fatty acids represent an interesting class of minor components, which has been overlooked so far. In this work, an untargeted approach based on liquid-chromatography coupled to a high-resolution mass spectrometry and a dedicated structure-based workflow for raw data interpretation was employed for the characterization of fatty acids from hemp inflorescences. A simple method, without any chemical derivatization, was developed for extraction and characterization of fatty acids leading to the tentative identification of 39 fatty acid species in the five hemp samples. A quantitative analysis on the untargeted data was initially performed, using peak areas as surrogate of analyte abundance for relative quantitation. Five fatty acids resulted the most abundant in all hemp samples, with ca. 90% of the total peak area. For these compounds a targeted quantitative method was validated, indicating that the most abundant ones were linolenic acid (1.39–7.95 mg g-1) and linoleic acid (1.04–7.87 mg g-1), followed by palmitic acid (3.74–6.08 mg g-1), oleic acid (0.91–4.73 mg g-1) and stearic acid (0.64–2.25 mg g-1).
Susy Piovesana; Sara Elsa Aita; Giuseppe Cannazza; Anna Laura Capriotti; Chiara Cavaliere; Andrea Cerrato; Paolo Guarnaccia; Carmela Maria Montone; Aldo Laganà. In-depth cannabis fatty acid profiling by ultra-high performance liquid chromatography coupled to high resolution mass spectrometry. Talanta 2021, 228, 122249 .
AMA StyleSusy Piovesana, Sara Elsa Aita, Giuseppe Cannazza, Anna Laura Capriotti, Chiara Cavaliere, Andrea Cerrato, Paolo Guarnaccia, Carmela Maria Montone, Aldo Laganà. In-depth cannabis fatty acid profiling by ultra-high performance liquid chromatography coupled to high resolution mass spectrometry. Talanta. 2021; 228 ():122249.
Chicago/Turabian StyleSusy Piovesana; Sara Elsa Aita; Giuseppe Cannazza; Anna Laura Capriotti; Chiara Cavaliere; Andrea Cerrato; Paolo Guarnaccia; Carmela Maria Montone; Aldo Laganà. 2021. "In-depth cannabis fatty acid profiling by ultra-high performance liquid chromatography coupled to high resolution mass spectrometry." Talanta 228, no. : 122249.
Polyhydroxyalkanoates (PHAs) are well-known biodegradable plastics produced by various bacterial strains, whose major drawback is constituted by the high cost of their synthesis. Producing PHAs from mixed microbial cultures and employing organic wastes as a carbon source allows us to both reduce cost and valorize available renewable resources, such as food waste and sewage sludge. However, different types of pollutants, originally contained in organic matrices, could persist into the final product, thus compromising their safety. In this work, the exploitation of municipal wastes for PHA production is evaluated from the environmental and health safety aspect by determining the presence of polycyclic aromatic hydrocarbons (PAHs) in both commercial and waste-based PHA samples. Quantification of PAHs by gas chromatography-mass spectrometry on 24 PHA samples obtained in different conditions showed very low contamination levels, in the range of ppb to a few ppm. Moreover, the contaminant content seems to be dependent on the type of PHA stabilization and extraction, but independent from the type of feedstock. Commercial PHA derived from crops, selected for comparison, showed PAH content comparable to that detected in PHAs derived from organic fraction of municipal solid waste. Although there is no specific regulation on PAH maximum levels in PHAs, detected concentrations were consistently lower than threshold limit values set by regulation and guidelines for similar materials and/or applications. This suggests that the use of organic waste as substrate for PHA production is safe for both the human health and the environment.
Chiara Cavaliere; Anna Capriotti; Andrea Cerrato; Laura Lorini; Carmela Montone; Francesco Valentino; Aldo Laganà; Mauro Majone. Identification and Quantification of Polycyclic Aromatic Hydrocarbons in Polyhydroxyalkanoates Produced from Mixed Microbial Cultures and Municipal Organic Wastes at Pilot Scale. Molecules 2021, 26, 539 .
AMA StyleChiara Cavaliere, Anna Capriotti, Andrea Cerrato, Laura Lorini, Carmela Montone, Francesco Valentino, Aldo Laganà, Mauro Majone. Identification and Quantification of Polycyclic Aromatic Hydrocarbons in Polyhydroxyalkanoates Produced from Mixed Microbial Cultures and Municipal Organic Wastes at Pilot Scale. Molecules. 2021; 26 (3):539.
Chicago/Turabian StyleChiara Cavaliere; Anna Capriotti; Andrea Cerrato; Laura Lorini; Carmela Montone; Francesco Valentino; Aldo Laganà; Mauro Majone. 2021. "Identification and Quantification of Polycyclic Aromatic Hydrocarbons in Polyhydroxyalkanoates Produced from Mixed Microbial Cultures and Municipal Organic Wastes at Pilot Scale." Molecules 26, no. 3: 539.
Among the bioactive compounds present in extra-virgin olive oil, polar lipids and free fatty acids are minor compounds with well-known nutritional values and have been studied for traceability and adulteration investigations as well. In the present paper, the simultaneous characterization of polar lipids and free fatty acids in a pool of fifteen EVOO samples was achieved by means of reversed phase C18 analysis coupled to negative polarity high-resolution mass spectrometry. A total of 24 polar lipids, comprising 19 phospholipids and 5 sulfolipids, and 27 free fatty acids were tentatively identified, including several odd-chain and very long-chain fatty acids at trace levels. Moreover, a one-month study of lipid degradation on simulated storage conditions was carried out thanks to the set-up of a dedicated approach for degradation product analysis which was implemented of Compound Discoverer software. By virtue of the customized data processing workflow, more than forty compounds were tentatively identified, including compounds deriving from hydrolysis and oxidation reactions. Finally, by analysis of peak area trends, phosphoester hydrolyses of polar heads of phospholipids emerged as the fastest reactions, followed by glycerol ester hydrolyses and oxidative processes.
Anna Laura Capriotti; Andrea Cerrato; Sara Elsa Aita; Carmela Maria Montone; Susy Piovesana; Aldo Laganà; Chiara Cavaliere. Degradation of the polar lipid and fatty acid molecular species in extra virgin olive oil during storage based on shotgun lipidomics. Journal of Chromatography A 2021, 1639, 461881 .
AMA StyleAnna Laura Capriotti, Andrea Cerrato, Sara Elsa Aita, Carmela Maria Montone, Susy Piovesana, Aldo Laganà, Chiara Cavaliere. Degradation of the polar lipid and fatty acid molecular species in extra virgin olive oil during storage based on shotgun lipidomics. Journal of Chromatography A. 2021; 1639 ():461881.
Chicago/Turabian StyleAnna Laura Capriotti; Andrea Cerrato; Sara Elsa Aita; Carmela Maria Montone; Susy Piovesana; Aldo Laganà; Chiara Cavaliere. 2021. "Degradation of the polar lipid and fatty acid molecular species in extra virgin olive oil during storage based on shotgun lipidomics." Journal of Chromatography A 1639, no. : 461881.
Native peptides from sea bass muscle were analyzed by two different approaches: medium-sized peptides by peptidomics analysis, whereas short peptides by suspect screening analysis employing an inclusion list of exact m/z values of all possible amino acid combinations (from 2 up to 4). The method was also extended to common post-translational modifications potentially interesting in food analysis, as well as non-proteolytic aminoacyl derivatives, which are well-known taste-active building blocks in pseudo-peptides. The medium-sized peptides were identified by de novo and combination of de novo and spectra matching to a protein sequence database, with up to 4077 peptides (2725 modified) identified by database search and 2665 peptides (223 modified) identified by de novo only; 102 short peptide sequences were identified (with 12 modified ones), and most of them had multiple reported bioactivities. The method can be extended to any peptide mixture, either endogenous or by protein hydrolysis, from other food matrices.
Andrea Cerrato; Sara Elsa Aita; Chiara Cavaliere; Aldo Laganà; Carmela Maria Montone; Susy Piovesana; Riccardo Zenezini Chiozzi; Anna Laura Capriotti. Comprehensive identification of native medium-sized and short bioactive peptides in sea bass muscle. Food Chemistry 2020, 343, 128443 .
AMA StyleAndrea Cerrato, Sara Elsa Aita, Chiara Cavaliere, Aldo Laganà, Carmela Maria Montone, Susy Piovesana, Riccardo Zenezini Chiozzi, Anna Laura Capriotti. Comprehensive identification of native medium-sized and short bioactive peptides in sea bass muscle. Food Chemistry. 2020; 343 ():128443.
Chicago/Turabian StyleAndrea Cerrato; Sara Elsa Aita; Chiara Cavaliere; Aldo Laganà; Carmela Maria Montone; Susy Piovesana; Riccardo Zenezini Chiozzi; Anna Laura Capriotti. 2020. "Comprehensive identification of native medium-sized and short bioactive peptides in sea bass muscle." Food Chemistry 343, no. : 128443.
The review describes the state of the art of phenolic characterization in food by liquid chromatography and mass spectrometry. From conventional targeted analysis, a special attention was devoted to metabolomics-based strategies, which are becoming increasingly popular in the characterization of phenolic compounds. Most works in the field exploit the profiling approach by annotation of full scan high resolution mass spectrometric data. To improve the confidence, the use of tandem and multistage mass spectrometry is emerging as a valuable strategy which can provide more insight in the structure and help differentiating the many isomeric compounds which are typical of this class. The efficiency, however, is strictly connected with data handling and bioinformatics to search databases and match product ion spectra. The different approaches, from profiling, through suspect screening to untargeted analysis, are described with a discussion on the limitations of each approach and future developments needed to improve identification confidence.
Susy Piovesana; Chiara Cavaliere; Andrea Cerrato; Carmela Maria Montone; Aldo Laganà; Anna Laura Capriotti. Developments and pitfalls in the characterization of phenolic compounds in food: From targeted analysis to metabolomics-based approaches. TrAC Trends in Analytical Chemistry 2020, 133, 116083 .
AMA StyleSusy Piovesana, Chiara Cavaliere, Andrea Cerrato, Carmela Maria Montone, Aldo Laganà, Anna Laura Capriotti. Developments and pitfalls in the characterization of phenolic compounds in food: From targeted analysis to metabolomics-based approaches. TrAC Trends in Analytical Chemistry. 2020; 133 ():116083.
Chicago/Turabian StyleSusy Piovesana; Chiara Cavaliere; Andrea Cerrato; Carmela Maria Montone; Aldo Laganà; Anna Laura Capriotti. 2020. "Developments and pitfalls in the characterization of phenolic compounds in food: From targeted analysis to metabolomics-based approaches." TrAC Trends in Analytical Chemistry 133, no. : 116083.
Due to the rapidly increasing resistance to conventional antibiotics, antimicrobial peptides are emerging as promising novel drug candidates. In this study, peptide fragments were obtained from yellowfin tuna muscle by simulated gastrointestinal digestion, and their antimicrobial activity towards Gram-positive and Gram-negative bacteria was investigated. In particular, the antimicrobial activity of both medium- and short-sized peptides was investigated by using two dedicated approaches. Medium-sized peptides were purified by solid phase extraction on C18, while short peptides were purified thanks to a graphitized carbon black sorbent. For medium-sized peptide characterization, a peptidomic strategy based on shotgun proteomics analysis was employed, and identification was achieved by matching protein sequence database by homology, as yellowfin tuna is a non-model organism, leading to the identification of 403 peptides. As for short peptide sequences, an untargeted suspect screening approach was carried out by means of an inclusion list presenting the exact mass to charge ratios (m/z) values for all di-, tri- and tetrapeptides. In total, 572 short sequences were identified thanks to a customized workflow dedicated to short peptide analysis implemented on Compound Discoverer software.
Andrea Cerrato; Anna Capriotti; Federico Capuano; Chiara Cavaliere; Angela Montone; Carmela Montone; Susy Piovesana; Riccardo Zenezini Chiozzi; Aldo Laganà. Identification and Antimicrobial Activity of Medium-Sized and Short Peptides from Yellowfin Tuna (Thunnus albacares) Simulated Gastrointestinal Digestion. Foods 2020, 9, 1185 .
AMA StyleAndrea Cerrato, Anna Capriotti, Federico Capuano, Chiara Cavaliere, Angela Montone, Carmela Montone, Susy Piovesana, Riccardo Zenezini Chiozzi, Aldo Laganà. Identification and Antimicrobial Activity of Medium-Sized and Short Peptides from Yellowfin Tuna (Thunnus albacares) Simulated Gastrointestinal Digestion. Foods. 2020; 9 (9):1185.
Chicago/Turabian StyleAndrea Cerrato; Anna Capriotti; Federico Capuano; Chiara Cavaliere; Angela Montone; Carmela Montone; Susy Piovesana; Riccardo Zenezini Chiozzi; Aldo Laganà. 2020. "Identification and Antimicrobial Activity of Medium-Sized and Short Peptides from Yellowfin Tuna (Thunnus albacares) Simulated Gastrointestinal Digestion." Foods 9, no. 9: 1185.
Phytocannabinoids are a broad class of compounds uniquely synthesized by the various strains of Cannabis sativa. Up to date, most investigation on phytocannabinoids have been addressed to the most abundant species, Δ9-tetrahydrocannabinol and cannabidiol, for their well-known wide range of pharmaceutical activities. However, in the recent years a large number of minor constituents have been reported, whose role in cannabis pharmacological effects is of current scientific interest. With the purpose of gaining knowledge on major and minor species and furnishing a strategy for their untargeted analysis, in this study we present an innovative approach for comprehensively identifying phytocannabinoids based on high-resolution mass spectrometry in negative ion mode, which allows discrimination of the various isomeric species. For a faster and more reliable manual validation of the tandem mass spectra of known and still unknown species, an extensive database of phytocannabinoid derivatives was compiled and implemented on Compound Discoverer software for the setup of a dedicated data analysis tool. The method was applied to extracts of the Italian FM-2 medicinal cannabis, resulting in the identification of 121 phytocannabinoids, which is the highest number ever reported in a single analysis. Among those, many known and still unknown unconventional phytocannabinoids have been tentatively identified, another piece in the puzzle of unravelling the many uncharted applications of this matrix.
Carmela Maria Montone; Andrea Cerrato; Bruno Botta; Giuseppe Cannazza; Anna Laura Capriotti; Chiara Cavaliere; Cinzia Citti; Francesca Ghirga; Susy Piovesana; Aldo Laganà. Improved identification of phytocannabinoids using a dedicated structure-based workflow. Talanta 2020, 219, 121310 .
AMA StyleCarmela Maria Montone, Andrea Cerrato, Bruno Botta, Giuseppe Cannazza, Anna Laura Capriotti, Chiara Cavaliere, Cinzia Citti, Francesca Ghirga, Susy Piovesana, Aldo Laganà. Improved identification of phytocannabinoids using a dedicated structure-based workflow. Talanta. 2020; 219 ():121310.
Chicago/Turabian StyleCarmela Maria Montone; Andrea Cerrato; Bruno Botta; Giuseppe Cannazza; Anna Laura Capriotti; Chiara Cavaliere; Cinzia Citti; Francesca Ghirga; Susy Piovesana; Aldo Laganà. 2020. "Improved identification of phytocannabinoids using a dedicated structure-based workflow." Talanta 219, no. : 121310.
Short peptides are of extreme interest in clinical and food research fields, nevertheless they still represent a crucial analytical issue. The main aim of this paper was the development of an analytical platform for a considerable advancement in short peptides identification. For the first time, short sequences presenting both natural and post-translationally modified amino acids were comprehensively studied thanks to the generation of specific databases. Short peptide databases had a dual purpose. First, they were employed as inclusion lists for a suspect screening mass-spectrometric analysis, overcoming the limits of data dependent acquisition mode and allowing the fragmentation of such low-abundance substances. Moreover, the databases were implemented in Compound Discoverer 3.0, a software dedicated to the analysis of short molecules, for the creation of a data processing workflow specifically dedicated to short peptide tentative identification. For this purpose, a detailed study of short peptide fragmentation pathways was carried out for the first time. The proposed method was applied to the study of short peptide sequences in enriched urine samples and led to the tentative identification more than 200 short natural and modified short peptides, the highest number ever reported.
Andrea Cerrato; Sara Elsa Aita; Anna Laura Capriotti; Chiara Cavaliere; Carmela Maria Montone; Aldo Laganà; Susy Piovesana. A new opening for the tricky untargeted investigation of natural and modified short peptides. Talanta 2020, 219, 121262 .
AMA StyleAndrea Cerrato, Sara Elsa Aita, Anna Laura Capriotti, Chiara Cavaliere, Carmela Maria Montone, Aldo Laganà, Susy Piovesana. A new opening for the tricky untargeted investigation of natural and modified short peptides. Talanta. 2020; 219 ():121262.
Chicago/Turabian StyleAndrea Cerrato; Sara Elsa Aita; Anna Laura Capriotti; Chiara Cavaliere; Carmela Maria Montone; Aldo Laganà; Susy Piovesana. 2020. "A new opening for the tricky untargeted investigation of natural and modified short peptides." Talanta 219, no. : 121262.
Chestnut seeds are used for fresh consumption and for the industrial preparation of derivatives, such as chestnut flour. During industrial processing, large amounts of by-products are generally produced, such as leaves, flowers, shells and burs. In the present study, chestnut shells were extracted by boiling water in order to obtain polyphenol-rich extracts. Moreover, for the removal or non-phenolic compounds, a separation by preparative reverse phase chromatography in ten fractions was carried out. The richest fractions in terms of phenolic content were characterized by means of untargeted high-resolution mass spectrometric analysis together with a dedicated and customized data processing workflow. A total of 243 flavonoids, phenolic acids, proanthocyanidins and ellagitannins were tentatively identified in the five richest fractions. Due its high phenolic content (450.03 µg GAE per mg of fraction), one tumor cell line (DU 145) and one normal prostate epithelial cell line (PNT2) were exposed to increasing concentration of fraction 3 dry extract for 24, 48 and 72 h. Moreover, for DU 145 cell lines, increase of apoptotic cells and perturbation of cell cycle was demonstrated for the same extract. Those outcomes suggest that chestnut industrial by-products could be potentially employed as a source of bioresources.
Nunzio Antonio Cacciola; Andrea Cerrato; Anna Laura Capriotti; Chiara Cavaliere; Maria D’Apolito; Carmela Maria Montone; Susy Piovesana; Giuseppe Squillaci; Gianfranco Peluso; Aldo Laganà. Untargeted Characterization of Chestnut (Castanea sativa Mill.) Shell Polyphenol Extract: A Valued Bioresource for Prostate Cancer Cell Growth Inhibition. Molecules 2020, 25, 2730 .
AMA StyleNunzio Antonio Cacciola, Andrea Cerrato, Anna Laura Capriotti, Chiara Cavaliere, Maria D’Apolito, Carmela Maria Montone, Susy Piovesana, Giuseppe Squillaci, Gianfranco Peluso, Aldo Laganà. Untargeted Characterization of Chestnut (Castanea sativa Mill.) Shell Polyphenol Extract: A Valued Bioresource for Prostate Cancer Cell Growth Inhibition. Molecules. 2020; 25 (12):2730.
Chicago/Turabian StyleNunzio Antonio Cacciola; Andrea Cerrato; Anna Laura Capriotti; Chiara Cavaliere; Maria D’Apolito; Carmela Maria Montone; Susy Piovesana; Giuseppe Squillaci; Gianfranco Peluso; Aldo Laganà. 2020. "Untargeted Characterization of Chestnut (Castanea sativa Mill.) Shell Polyphenol Extract: A Valued Bioresource for Prostate Cancer Cell Growth Inhibition." Molecules 25, no. 12: 2730.
Protein tyrosine O-sulfation is an important post-translational modification, as it has been correlated to inflammation, virus infection, and signal pathways. Nevertheless, methods for the characterization of protein sulfation by sulfopeptide enrichment are currently limited. In this Article, two standard compounds, representative of mono- and disulfated peptides, were used to compare the enrichment capabilities of five sorbent materials: two commercial weak anion-exchange mixed-mode sorbents (Strata X-AW and Oasis WAX) and three phosphopeptide enrichment materials based on affinity chromatography to either immobilized metals (IMAC) or metal oxides, i.e., Fe3+, TiO2, or Ti4+. The sulfopeptides were analyzed by ultrahigh-performance liquid chromatography (UHPLC) multiple-reaction monitoring analysis and were stable under all the tested experimental conditions. Recoveries of the enrichment step from spiked bovine serum albumin digests were >80% for the commercial Fe-IMAC kit and the Strata X-AW sorbent. Shotgun proteomics was used on the same samples to evaluate the selectivity, calculated as the number of coenriched peptides, and it was found to be better for the Fe-IMAC kit. Therefore, the Fe-IMAC protocol was embedded in a shotgun-proteomics workflow and applied to serum spiked with the sulfopeptides before protein dephosphorylation and digestion. The recovery of the entire analytical workflow was 20%, which was compatible with previous data on TiO2 phosphopeptide enrichment. Despite the potential, no sulfopeptide was confidently identified in serum digests by conventional shotgun proteomics, probably due to very low abundance of native sulfoproteins, poor ionization efficiency of sulfopeptides in the positive mode, and lack of unambiguous sulfopeptide identification by bioinformatics software. In this context, the use of negative-ionization mode with high-resolution mass spectrometry appeared promising to improve the sensibility and allow sulfopeptide identification in complex samples.
Anna Laura Capriotti; Andrea Cerrato; Aldo Laganà; Carmela Maria Montone; Susy Piovesana; Riccardo Zenezini Chiozzi; Chiara Cavaliere. Development of a Sample-Preparation Workflow for Sulfopeptide Enrichment: From Target Analysis to Challenges in Shotgun Sulfoproteomics. Analytical Chemistry 2020, 92, 7964 -7971.
AMA StyleAnna Laura Capriotti, Andrea Cerrato, Aldo Laganà, Carmela Maria Montone, Susy Piovesana, Riccardo Zenezini Chiozzi, Chiara Cavaliere. Development of a Sample-Preparation Workflow for Sulfopeptide Enrichment: From Target Analysis to Challenges in Shotgun Sulfoproteomics. Analytical Chemistry. 2020; 92 (11):7964-7971.
Chicago/Turabian StyleAnna Laura Capriotti; Andrea Cerrato; Aldo Laganà; Carmela Maria Montone; Susy Piovesana; Riccardo Zenezini Chiozzi; Chiara Cavaliere. 2020. "Development of a Sample-Preparation Workflow for Sulfopeptide Enrichment: From Target Analysis to Challenges in Shotgun Sulfoproteomics." Analytical Chemistry 92, no. 11: 7964-7971.
The determination of phospholipids in olive oil is challenging due to their low concentration. For this reason, a comparison of two solid phase extraction procedures, namely weak anionic exchange (WAX) and graphitized carbon black (GCB), is presented for the enrichment of phospholipids. Analyses were performed by liquid chromatography-high resolution mass spectrometry (LC-HRMS) and lipids were identified by Lipostar software. Compared to the WAX solid phase extraction, GCB demonstrated the best performance and provided 82 identified phospholipids vs only 32. The final method was validated for some representative phospholipids, showing good repeatability and recovery (63–101%). High sensitivity was reached, with detection limits in the range 9–36 ng g−1, never reported before for phospholipids in olive oil. A semi-quantitative analysis indicated phosphatidic acids and phosphatidylglycerols as the most abundant species, both in number and concentrations. The GCB-LC-HRMS-Lipostar platform can be successfully applied for a comprehensive polar lipidomic characterization of olive oils.
Michela Antonelli; Barbara Benedetti; Chiara Cavaliere; Andrea Cerrato; Carmela Maria Montone; Susy Piovesana; Aldo Lagana; Anna Laura Capriotti. Phospholipidome of extra virgin olive oil: Development of a solid phase extraction protocol followed by liquid chromatography–high resolution mass spectrometry for its software-assisted identification. Food Chemistry 2020, 310, 125860 .
AMA StyleMichela Antonelli, Barbara Benedetti, Chiara Cavaliere, Andrea Cerrato, Carmela Maria Montone, Susy Piovesana, Aldo Lagana, Anna Laura Capriotti. Phospholipidome of extra virgin olive oil: Development of a solid phase extraction protocol followed by liquid chromatography–high resolution mass spectrometry for its software-assisted identification. Food Chemistry. 2020; 310 ():125860.
Chicago/Turabian StyleMichela Antonelli; Barbara Benedetti; Chiara Cavaliere; Andrea Cerrato; Carmela Maria Montone; Susy Piovesana; Aldo Lagana; Anna Laura Capriotti. 2020. "Phospholipidome of extra virgin olive oil: Development of a solid phase extraction protocol followed by liquid chromatography–high resolution mass spectrometry for its software-assisted identification." Food Chemistry 310, no. : 125860.
Microalgae have recently become a popular functional food due to their health benefits. Sulfolipids, a class of substances abundant in this matrix, have been reported to have interesting bioactivities, such as anti-carcinogenic activity. However, despite the potential interest in sulfolipids, a dedicated analytical method for their characterization is currently lacking but would significantly increase the coverage of sulfolipids with respect to the direct lipidomic analysis. To achieve this goal, in this work a procedure, based on graphitized carbon black solid phase extraction, was developed for clean-up and enrichment of sulfolipids (sulfoquinovosyldiacylglycerols and sulfoquinovosylmonoacylglycerols) and it was applied to spirulina (Arthrospira platensis) microalgae. A careful study of the solid phase extraction conditions was performed, first to maximize the recovery of reference standards, then to increase the total number of identified sulfolipids from the spirulina lipid extract. All samples were analysed by ultra-high performance liquid chromatography coupled to high resolution mass spectrometry and lipids were tentatively identified by Lipostar, for a reliable lipid structure assignment. The developed method was compared to the direct lipidomic analysis without enrichment, to establish the enrichment efficiency in terms of number of identifications. From the comparison, the enrichment procedure proved better and allowed the tentative identification of 199 sulfolipids, which is the largest number reported so far for the Arthrospira platensis species. The described method was validated in terms of precision, accuracy, recovery, limit of quantitation and detection for two sulfolipids. Finally, a relative lipid quantitation based on peak area was carried out on the microalgae sample, which indicated nine abundant sulfolipids as representing ca. 60% of sulfolipids in spirulina microalgae.
Michela Antonelli; Barbara Benedetti; Chiara Cavaliere; Andrea Cerrato; Giorgia La Barbera; Carmela Maria Montone; Susy Piovesana; Aldo Laganà. Enrichment procedure based on graphitized carbon black and liquid chromatography-high resolution mass spectrometry for elucidating sulfolipids composition of microalgae. Talanta 2019, 205, 120162 .
AMA StyleMichela Antonelli, Barbara Benedetti, Chiara Cavaliere, Andrea Cerrato, Giorgia La Barbera, Carmela Maria Montone, Susy Piovesana, Aldo Laganà. Enrichment procedure based on graphitized carbon black and liquid chromatography-high resolution mass spectrometry for elucidating sulfolipids composition of microalgae. Talanta. 2019; 205 ():120162.
Chicago/Turabian StyleMichela Antonelli; Barbara Benedetti; Chiara Cavaliere; Andrea Cerrato; Giorgia La Barbera; Carmela Maria Montone; Susy Piovesana; Aldo Laganà. 2019. "Enrichment procedure based on graphitized carbon black and liquid chromatography-high resolution mass spectrometry for elucidating sulfolipids composition of microalgae." Talanta 205, no. : 120162.
The chemical composition of Cannabis sativa L. has been extensively investigated for several years; nevertheless, a detailed lipidome characterization is completely lacking in the literature. To achieve this goal, an extraction and enrichment procedure was developed for the characterization of phospholipids and sulfolipids. Firstly, a study on the solid-liquid extraction was performed, to maximize the recovery of the considered lipids; the best procedure consisted of a simple extraction with a mixture of methanol and chloroform (1:1, v/v). The hemp extracts were analyzed by ultra-high-performance liquid chromatography coupled to high-resolution mass spectrometry and lipids were tentatively identified by Lipostar. To improve the number of identifications, an enrichment method, based on graphitized carbon black solid phase extraction, was evaluated to fractionate phospholipids and sulfolipids into separate eluates. Recovery and matrix effects of the procedure were determined on a mixture of standard lipids, containing representative compounds for each considered lipid class. The optimized method allowed the tentative identification of 189 lipids, including 51 phospholipids and 80 sulfolipids, in the first and second fractions, respectively. The detection of only 6 sulfolipids in the first fraction and 9 phospholipids in the second fraction proved the efficacy of the fractionation method, which also allowed the number of lipid identifications to be increased compared to the same procedure without enrichment, which scored 100 lipids. Finally, a semi-quantitative analysis permitted the hemp polar lipidome to be characterized. The results of this study allow knowledge of the hemp chemical composition to be improved with a detailed description of its phospho- and sulfolipid profiles.
Michela Antonelli; Barbara Benedetti; Giuseppe Cannazza; Andrea Cerrato; Cinzia Citti; Carmela Maria Montone; Susy Piovesana; Aldo Laganà. New insights in hemp chemical composition: a comprehensive polar lipidome characterization by combining solid phase enrichment, high-resolution mass spectrometry, and cheminformatics. Analytical and Bioanalytical Chemistry 2019, 412, 413 -423.
AMA StyleMichela Antonelli, Barbara Benedetti, Giuseppe Cannazza, Andrea Cerrato, Cinzia Citti, Carmela Maria Montone, Susy Piovesana, Aldo Laganà. New insights in hemp chemical composition: a comprehensive polar lipidome characterization by combining solid phase enrichment, high-resolution mass spectrometry, and cheminformatics. Analytical and Bioanalytical Chemistry. 2019; 412 (2):413-423.
Chicago/Turabian StyleMichela Antonelli; Barbara Benedetti; Giuseppe Cannazza; Andrea Cerrato; Cinzia Citti; Carmela Maria Montone; Susy Piovesana; Aldo Laganà. 2019. "New insights in hemp chemical composition: a comprehensive polar lipidome characterization by combining solid phase enrichment, high-resolution mass spectrometry, and cheminformatics." Analytical and Bioanalytical Chemistry 412, no. 2: 413-423.