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Seaweeds are a marine source rich in potentially bioactive components, and therefore have attracted attention since the middle of the twentieth century. Accurate and objective assessment of the intake of seaweeds to study their health effects is hampered by a lack of validated intake biomarkers. In this three-armed, randomized, cross-over study, an untargeted metabolomics approach was applied for discovering novel intake biomarkers. Twenty healthy participants (9 men and 11 women) were provided each of three test meals in a randomized order: 5 g of Laminaria digitate (LD), 5 g of Undaria pinnatifida (UP), or a control meal with energy-adjusted pea protein. Four urine samples and a 24 h pooled urine were collected along with blood samples at seven time-points. All samples were profiled by LC-ESI-QTOF-MS and the data were analyzed by univariate analysis and excretion kinetics to select putative intake biomarkers. In total, four intake biomarkers were selected from urine samples. They were identified as hydroxyl-dihydrocoumarin at Level III, loliolid glucuronide at level I, and isololiolid glucuronide at level II, while the last one remains unknown. Further identification and validation of these biomarkers by a cross-sectional study is essential to assess their specificity and robustness.
Muyao Xi; Lars Ove Dragsted; Mikkel Tullin; Madeleine Ernst; Nazikussabah Zaharudin; Giorgia La Barbera. Discovery of Urinary Biomarkers of Seaweed Intake Using Untargeted LC–MS Metabolomics in a Three-Way Cross-Over Human Study. Metabolites 2020, 11, 11 .
AMA StyleMuyao Xi, Lars Ove Dragsted, Mikkel Tullin, Madeleine Ernst, Nazikussabah Zaharudin, Giorgia La Barbera. Discovery of Urinary Biomarkers of Seaweed Intake Using Untargeted LC–MS Metabolomics in a Three-Way Cross-Over Human Study. Metabolites. 2020; 11 (1):11.
Chicago/Turabian StyleMuyao Xi; Lars Ove Dragsted; Mikkel Tullin; Madeleine Ernst; Nazikussabah Zaharudin; Giorgia La Barbera. 2020. "Discovery of Urinary Biomarkers of Seaweed Intake Using Untargeted LC–MS Metabolomics in a Three-Way Cross-Over Human Study." Metabolites 11, no. 1: 11.
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.
Polyphenols are a broad class of plant secondary metabolites which carry out several biological functions for plant growth and protection and are of great interest as nutraceuticals for their antioxidant properties. However, due to their structural variability and complexity, the mass-spectrometric analysis of polyphenol content in plant matrices is still an issue. In this work, a novel approach for the identification of several classes of polyphenol derivatives based on ultra-high performance liquid chromatography coupled to high-resolution mass spectrometry was developed. First, mass-spectrometric parameters were optimized in order to obtain a large set of diagnostic product ions for their high-confidence identification. The software Compound Discoverer 3.0 was then implemented with a comprehensive database of 45,567 polyphenol derivatives and with mass-spectrometric data for their building blocks, resulting in a specific tool for the semi-automatic identification of flavonoids, anthocyanins, ellagitannins, proanthocyanidins and phenolic acids. The method was then applied to the identification of polyphenols in industrial hemp (Cannabis sativa), a matrix whose use is recently spreading for pharmaceutical and nutraceutical purposes, resulting in the identification of 147 compounds belonging to the classes of flavonoids, proanthocyanidins and phenolic acids. The proposed method is applicable to the polyphenol profiling of any plant matrix and it is not dependent on data in the literature for their identification, allowing the discovery of compounds which have been never identified before.
Andrea Cerrato; Giuseppe Cannazza; Anna Laura Capriotti; Cinzia Citti; Giorgia LA Barbera; Aldo Laganà; Carmela Maria Montone; Susy Piovesana; Chiara Cavaliere. A new software-assisted analytical workflow based on high-resolution mass spectrometry for the systematic study of phenolic compounds in complex matrices. Talanta 2019, 209, 120573 .
AMA StyleAndrea Cerrato, Giuseppe Cannazza, Anna Laura Capriotti, Cinzia Citti, Giorgia LA Barbera, Aldo Laganà, Carmela Maria Montone, Susy Piovesana, Chiara Cavaliere. A new software-assisted analytical workflow based on high-resolution mass spectrometry for the systematic study of phenolic compounds in complex matrices. Talanta. 2019; 209 ():120573.
Chicago/Turabian StyleAndrea Cerrato; Giuseppe Cannazza; Anna Laura Capriotti; Cinzia Citti; Giorgia LA Barbera; Aldo Laganà; Carmela Maria Montone; Susy Piovesana; Chiara Cavaliere. 2019. "A new software-assisted analytical workflow based on high-resolution mass spectrometry for the systematic study of phenolic compounds in complex matrices." Talanta 209, no. : 120573.
When drug nanocarriers enter a physiological environment, their surface gets coated by a dynamic biomolecular corona (BMC) mainly constituted by proteins. Although a deep investigation has been performed on the composition of BMC in terms of proteins, scarce attention has been posed to low molecular weight metabolites present in human plasma. In this work, for the first time, the investigation of the BMC of liposomal nanoparticles (NPs) constituted by 1,2-dioleoyl-3-trimethylammonium-propane polar lipid has been carried out by an ultra-high performance liquid chromatography coupled to high-resolution mass spectrometry based untargeted metabolomics approach. Compounds were tentatively identified based on matches with online databases and comparison of MS/MS spectra with available spectral libraries. Moreover, a comparison of three metabolite extraction strategies, including an ultrafiltration membrane based protocol, a methanol extraction based protocol, and Wessel & Flügge protocol, was performed. Methanol extraction procedure resulted in the widest metabolic coverage of liposomal NP BMC. A total of 193 metabolites has been tentatively identified, 166 of which belonged to the class of lipids including phospholipids, steroids, carnitines, fatty alcohols, diglycerides and fatty acids. The high abundance of lipids in the BMC can be explained by the adsorption of plasma lipoproteins onto liposome surface, confirming previous works on other kinds of NPs. Lipids are important bioactive molecules, which could impact NP circulation and uptake by cells. Extending the investigation of BMC beyond the protein corona and towards the “lipid corona” may be the keystone of a better understanding and control of NP fate in human body.
Giorgia La Barbera; Anna Laura Capriotti; Giulio Caracciolo; Chiara Cavaliere; Andrea Cerrato; Carmela Maria Montone; Susy Piovesana; Daniela Pozzi; Erica Quagliarini; Aldo Laganà. A comprehensive analysis of liposomal biomolecular corona upon human plasma incubation: The evolution towards the lipid corona. Talanta 2019, 209, 120487 .
AMA StyleGiorgia La Barbera, Anna Laura Capriotti, Giulio Caracciolo, Chiara Cavaliere, Andrea Cerrato, Carmela Maria Montone, Susy Piovesana, Daniela Pozzi, Erica Quagliarini, Aldo Laganà. A comprehensive analysis of liposomal biomolecular corona upon human plasma incubation: The evolution towards the lipid corona. Talanta. 2019; 209 ():120487.
Chicago/Turabian StyleGiorgia La Barbera; Anna Laura Capriotti; Giulio Caracciolo; Chiara Cavaliere; Andrea Cerrato; Carmela Maria Montone; Susy Piovesana; Daniela Pozzi; Erica Quagliarini; Aldo Laganà. 2019. "A comprehensive analysis of liposomal biomolecular corona upon human plasma incubation: The evolution towards the lipid corona." Talanta 209, no. : 120487.
The metaproteomic analysis of air particulate matter provides valuable information about the properties of bioaerosols in the atmosphere and their influence on climate and public health. In this work, a new method for the extraction and analysis of proteins in airborne particulate matter from quartz microfiber filters is developed. Different protein extraction procedures are tested to select the best extraction protocol based on protein recovery. The optimized method is tested for the extraction of proteins from spores of ubiquitous bacteria species and used for the metaproteomic characterization of filters from three work environments. In particular, ambient aerosol samples are collected in a composting plant, in a wastewater treatment plant, and in an agricultural holding. A total of 179, 15, 205, and 444 proteins are identified in composting plant, wastewater treatment plant, and agricultural holding, (cow stable and blending plant), respectively. In agreement with the major categories of primary biological aerosol particles, all identified proteins originated primarily from fungi, bacteria, and plants. The paper is the first metaproteomic study applied to bioaerosol samples collected in occupationally relevant environmental sites and, even though not aimed at monitoring the risk exposure of workers, it provides information on the possible exposure in the working environmental sites.
Susy Piovesana; Anna Laura Capriotti; Patrizia Foglia; Carmela Maria Montone; Giorgia LA Barbera; Riccardo Zenezini Chiozzi; Aldo Laganà; Chiara Cavaliere. Development of an Analytical Method for the Metaproteomic Investigation of Bioaerosol from Work Environments. PROTEOMICS 2019, 19, e1900152 .
AMA StyleSusy Piovesana, Anna Laura Capriotti, Patrizia Foglia, Carmela Maria Montone, Giorgia LA Barbera, Riccardo Zenezini Chiozzi, Aldo Laganà, Chiara Cavaliere. Development of an Analytical Method for the Metaproteomic Investigation of Bioaerosol from Work Environments. PROTEOMICS. 2019; 19 (23):e1900152.
Chicago/Turabian StyleSusy Piovesana; Anna Laura Capriotti; Patrizia Foglia; Carmela Maria Montone; Giorgia LA Barbera; Riccardo Zenezini Chiozzi; Aldo Laganà; Chiara Cavaliere. 2019. "Development of an Analytical Method for the Metaproteomic Investigation of Bioaerosol from Work Environments." PROTEOMICS 19, no. 23: e1900152.
Zearalenone (ZEN) is a nonsteroidal estrogenic mycotoxin produced by various Fusarium species and commonly occurring in corn and other cereals. Even though its acute toxicity is low, still the estrogenic activity of ZEN and metabolites is a matter of concern. In this work, a new magnetic molecularly imprinted polymer (mMIP) for the selective extraction of ZEN from cereal flours is presented. The mMIP was synthesized previously using quercetin as dummy template, and here we wanted to test its applicability to complex food samples. Analyte determination was carried out by high-performance liquid chromatography coupled to tandem mass spectrometry. The selectivity of the mMIP and the main validation method parameters were assessed. In particular, even in samples as complex as cereals, matrix effect was negligible. Although the mMIP showed cross-selectivity towards both ZEN-related and quercetin-related compounds, nonetheless ZEN recovery was > 95% for the two lower spiking levels, and the quantification limit was 0.14 ng g−1, i.e., ca. 500 times lower than the maximum limit fixed for most cereals by European law. Therefore, the material, also in comparison with a commercial sorbent, appears suitable for the application in food analysis, also to isolate ZEN at trace levels.
Chiara Cavaliere; Michela Antonelli; Andrea Cerrato; Giorgia La Barbera; Aldo Laganà; Michele Laus; Susy Piovesana; Anna Laura Capriotti. A Novel Magnetic Molecular Imprinted Polymer for Selective Extraction of Zearalenone from Cereal Flours before Liquid Chromatography-Tandem Mass Spectrometry Determination. Toxins 2019, 11, 493 .
AMA StyleChiara Cavaliere, Michela Antonelli, Andrea Cerrato, Giorgia La Barbera, Aldo Laganà, Michele Laus, Susy Piovesana, Anna Laura Capriotti. A Novel Magnetic Molecular Imprinted Polymer for Selective Extraction of Zearalenone from Cereal Flours before Liquid Chromatography-Tandem Mass Spectrometry Determination. Toxins. 2019; 11 (9):493.
Chicago/Turabian StyleChiara Cavaliere; Michela Antonelli; Andrea Cerrato; Giorgia La Barbera; Aldo Laganà; Michele Laus; Susy Piovesana; Anna Laura Capriotti. 2019. "A Novel Magnetic Molecular Imprinted Polymer for Selective Extraction of Zearalenone from Cereal Flours before Liquid Chromatography-Tandem Mass Spectrometry Determination." Toxins 11, no. 9: 493.
Short peptide sequences represent emerging analytes in a variety of fields, including biomarker discovery, but also a well-known analytical challenge in complex matrices, due to the low abundance, extensive suppression during MS analysis, and lack of workflows, as they cannot be identified by ordinary peptidomics strategies and coverage is extremely limited by metabolomics as well. In this context, in this work, a solid phase extraction method was developed for the cleanup and enrichment of dipeptides, tripeptides, and tetrapeptides in urine using graphitized carbon black Carbograph 4 as the sorbent. The method was first developed on analytical standards spiked in urine, with recoveries in the range of 60–100%. Then the method was applied to urine samples from healthy volunteers. The enriched urine samples were analyzed by ultrahigh performance liquid chromatography (UHPLC) using an orthogonal strategy in which both a reversed phase (RP) C18 column and a zwitterionic hydrophilic interaction liquid chromatography (HILIC) column were used, for better coverage of peptide polarity and improved detection of peptides. High-resolution mass spectra were acquired in data-dependent mode using a suspect screening strategy with inclusion list; peptides were identified by a semiautomated workflow for feature extraction, candidate mass filtering, and MS/MS spectra comparison with in silico mass spectra. The complementarity of the orthogonal separation strategy was confirmed by peptide identification, resulting in 101 peptides identified from the RP runs and 111 peptides from the HILIC runs, with 60 common identifications. The method is applicable to both hydrophobic and hydrophilic peptides. Peptides were stable over 2 h after collection and protease inhibitors were not necessary, as no formation of artifacts was observed.
Susy Piovesana; Anna Laura Capriotti; Andrea Cerrato; Carlo Crescenzi; Giorgia La Barbera; Aldo Laganà; Carmela Maria Montone; Chiara Cavaliere. Graphitized Carbon Black Enrichment and UHPLC-MS/MS Allow to Meet the Challenge of Small Chain Peptidomics in Urine. Analytical Chemistry 2019, 91, 11474 -11481.
AMA StyleSusy Piovesana, Anna Laura Capriotti, Andrea Cerrato, Carlo Crescenzi, Giorgia La Barbera, Aldo Laganà, Carmela Maria Montone, Chiara Cavaliere. Graphitized Carbon Black Enrichment and UHPLC-MS/MS Allow to Meet the Challenge of Small Chain Peptidomics in Urine. Analytical Chemistry. 2019; 91 (17):11474-11481.
Chicago/Turabian StyleSusy Piovesana; Anna Laura Capriotti; Andrea Cerrato; Carlo Crescenzi; Giorgia La Barbera; Aldo Laganà; Carmela Maria Montone; Chiara Cavaliere. 2019. "Graphitized Carbon Black Enrichment and UHPLC-MS/MS Allow to Meet the Challenge of Small Chain Peptidomics in Urine." Analytical Chemistry 91, no. 17: 11474-11481.
Anna Laura Capriotti; Giorgia La Barbera; Susy Piovesana. Recent Trends in Solid-Phase Extraction for Environmental, Food and Biological Sample Preparation. Chromatographia 2019, 82, 1119 -1120.
AMA StyleAnna Laura Capriotti, Giorgia La Barbera, Susy Piovesana. Recent Trends in Solid-Phase Extraction for Environmental, Food and Biological Sample Preparation. Chromatographia. 2019; 82 (8):1119-1120.
Chicago/Turabian StyleAnna Laura Capriotti; Giorgia La Barbera; Susy Piovesana. 2019. "Recent Trends in Solid-Phase Extraction for Environmental, Food and Biological Sample Preparation." Chromatographia 82, no. 8: 1119-1120.
An analytical method for determining seleno-methionine (SeMet), methyl-seleno-cysteine and seleno-cystine in extra-virgin olive oil (EVOO) was developed and validated. EVOO sample (15 g) was diluted with hexane, extracted with methanol/water 80:20 (v/v), and cleaned up by a reversed phase/strong cation exchange solid phase extraction. Analysis was performed by chiral hydrophilic interaction liquid chromatography-tandem mass spectrometry. Process efficiency ranged between 49 and 97% and trueness between 87 and 126%, with intermediate precision, expressed as standard deviation, lower than 10%. Method detection limits (MDLs) and method quantification limits (MQLs) were lower than 1 μg kg−1. Thirty-two EVOO samples from different Italian regions were analyzed for both total Se and single seleno-amino acids determination. Only l-SeMet was found at level MQL (0.2 μg kg−1)-1.42 μg kg−1 in ten samples, while total Se was in the range of MDL-9.1 μg kg−1. Concentration of l-SeMet (5–6% of total Se) and total Se correlated very well to each other (R2 = 0.995).
Susy Piovesana; Carmela Maria Montone; Michela Antonelli; Chiara Cavaliere; Giorgia La Barbera; Silvia Canepari; Roberto Samperi; Aldo Laganà; Anna Laura Capriotti. Investigation of free seleno-amino acids in extra-virgin olive oil by mixed mode solid phase extraction cleanup and enantioselective hydrophilic interaction liquid chromatography-tandem mass spectrometry. Food Chemistry 2019, 278, 17 -25.
AMA StyleSusy Piovesana, Carmela Maria Montone, Michela Antonelli, Chiara Cavaliere, Giorgia La Barbera, Silvia Canepari, Roberto Samperi, Aldo Laganà, Anna Laura Capriotti. Investigation of free seleno-amino acids in extra-virgin olive oil by mixed mode solid phase extraction cleanup and enantioselective hydrophilic interaction liquid chromatography-tandem mass spectrometry. Food Chemistry. 2019; 278 ():17-25.
Chicago/Turabian StyleSusy Piovesana; Carmela Maria Montone; Michela Antonelli; Chiara Cavaliere; Giorgia La Barbera; Silvia Canepari; Roberto Samperi; Aldo Laganà; Anna Laura Capriotti. 2019. "Investigation of free seleno-amino acids in extra-virgin olive oil by mixed mode solid phase extraction cleanup and enantioselective hydrophilic interaction liquid chromatography-tandem mass spectrometry." Food Chemistry 278, no. : 17-25.
This minireview is dedicated to the discussion of analytical methods based on magnetic solid-phase extraction for the investigation of different analyte classes in complex matrices. Magnetic solid-phase extraction represents one of the most exploited approaches for sample preparation, which benefits from the development of new materials and from the coupling with other purification and clean-up strategies. New materials are continuously described for the isolation and enrichment of a variety of compounds, from small molecules to biologic macromolecules. Such magnetic materials developed for magnetic solid-phase extraction are discussed in this minireview, spanning across different types of materials, from the more traditional magnetic nanoparticles functionalized with polymers, to molecularly imprinted polymers, but also graphene, carbon nanotubes, graphitized carbon black, metal organic frameworks, covalent organic frameworks, composite materials, biopolymers (polydopamine, chitosan), materials from wastes and natural products and the newly introduced knitting aromatic polymers. The magnetic solid-phase extraction methods are collected from the recent literature and organized in sections based on the target analyte classes, which include drugs, endocrine-disrupting compounds, pesticides, polycyclic aromatic hydrocarbons, metals, toxins, peptides, proteins, metabolites and a final chapter dedicated to applications to other common pollutants, contaminants and multiresidue methods. A selection of recent applications and variations of the traditional magnetic solid-phase extraction protocols is discussed for food, environmental and biologic matrices. Finally, the compliance of magnetic solid-phase extraction with the principles of green analytical chemistry is also briefly discussed, with recent examples, indicating the use of waste or sustainable materials, development of green material preparations and reduction of organic solvents as the main strategies for future development of environmentally friendly magnetic solid-phase extraction methods.
Anna Laura Capriotti; Chiara Cavaliere; Giorgia LA Barbera; Carmela Maria Montone; Susy Piovesana; Aldo Laganà. Recent Applications of Magnetic Solid-phase Extraction for Sample Preparation. Chromatographia 2019, 82, 1251 -1274.
AMA StyleAnna Laura Capriotti, Chiara Cavaliere, Giorgia LA Barbera, Carmela Maria Montone, Susy Piovesana, Aldo Laganà. Recent Applications of Magnetic Solid-phase Extraction for Sample Preparation. Chromatographia. 2019; 82 (8):1251-1274.
Chicago/Turabian StyleAnna Laura Capriotti; Chiara Cavaliere; Giorgia LA Barbera; Carmela Maria Montone; Susy Piovesana; Aldo Laganà. 2019. "Recent Applications of Magnetic Solid-phase Extraction for Sample Preparation." Chromatographia 82, no. 8: 1251-1274.
Short peptides are important compounds in a variety of fields, including food and nutraceutical applications, but also biomarker discovery, bioactive peptide discovery and peptide drug separation. Despite the importance of short peptides, they are currently less studied than other peptides because of the lack of dedicated methods for their characterization. The method described in this paper comprises a combination of strategies to tackle the main limitations in short peptide analysis. In particular, in this work an untargeted peptidomic approach based on ultrahigh-performance liquid chromatography coupled to high-resolution mass spectrometry was developed for the identification of short peptides in cow milk samples. After milk defatting and precipitation, the sample was purified by cotton-hydrophilic interaction liquid chromatography (HILIC) micro tip in order to avoid suppression phenomena due to contaminants present in milk, such as carbohydrates. The sample was then separated by means of two chromatographic columns, with a complementary selectivity mechanism, namely reversed-phase C18 column and porous graphitic carbon (PGC). By this approach, the method allowed the separation and characterization of di-, tri- and tetrapeptides. A total of 57 and 41 peptides were identified by using a C18 and a PGC column, respectively; in particular, 31 were exclusively identified by using the C18 column, 15 unique peptides were identified by using the PGC column, while 26 were in common between the two data sets, demonstrating that the two columns have a different selectivity mechanism. The results indicated that an integrated approach may be appropriate to improve the separation of different peptides and increase the number of identifications because of the wide range of polarity of short peptides. The method allowed the untargeted identification of short peptides in milk, a complex matrix chosen as a representative real sample for method application, and provides complementary information to that accessible by ordinary peptidomics.
Carmela Maria Montone; Anna Laura Capriotti; Andrea Cerrato; Michela Antonelli; Giorgia LA Barbera; Susy Piovesana; Aldo Laganà; Chiara Cavaliere. Identification of bioactive short peptides in cow milk by high-performance liquid chromatography on C18 and porous graphitic carbon coupled to high-resolution mass spectrometry. Analytical and Bioanalytical Chemistry 2019, 411, 3395 -3404.
AMA StyleCarmela Maria Montone, Anna Laura Capriotti, Andrea Cerrato, Michela Antonelli, Giorgia LA Barbera, Susy Piovesana, Aldo Laganà, Chiara Cavaliere. Identification of bioactive short peptides in cow milk by high-performance liquid chromatography on C18 and porous graphitic carbon coupled to high-resolution mass spectrometry. Analytical and Bioanalytical Chemistry. 2019; 411 (15):3395-3404.
Chicago/Turabian StyleCarmela Maria Montone; Anna Laura Capriotti; Andrea Cerrato; Michela Antonelli; Giorgia LA Barbera; Susy Piovesana; Aldo Laganà; Chiara Cavaliere. 2019. "Identification of bioactive short peptides in cow milk by high-performance liquid chromatography on C18 and porous graphitic carbon coupled to high-resolution mass spectrometry." Analytical and Bioanalytical Chemistry 411, no. 15: 3395-3404.
Liquid chromatography coupled to low-resolution mass spectrometry (LRMS) has historically been a popular approach for compound quantitation. Recently, high-resolution mass spectrometry (HRMS) technical developments led to the introduction of new approaches for quantitative analysis. Whereas the performances of HRMS have been largely assessed for qualitative purposes, there are still questions about its suitability for quantitative analysis. Several papers on LRMS and HRMS comparison have been published; however, none of them was applied to polyphenol quantitation. In this work, a comparison between HRMS, operated in data-dependent acquisition mode, and LRMS, operated in selected-reaction-monitoring mode, was performed for polyphenol quantitation in wine. The two techniques were evaluated in terms of sensitivity, linearity range, matrix effect, and precision, showing the better performances of HRMS. The suitability of HRMS for quantitation purposes as well as qualitative screening makes HRMS the new technique of choice for both targeted and untargeted analysis.
Chiara Cavaliere; Michela Antonelli; Anna Laura Capriotti; Giorgia La Barbera; Carmela Maria Montone; Susy Piovesana; Aldo Laganà. A Triple Quadrupole and a Hybrid Quadrupole Orbitrap Mass Spectrometer in Comparison for Polyphenol Quantitation. Journal of Agricultural and Food Chemistry 2019, 67, 4885 -4896.
AMA StyleChiara Cavaliere, Michela Antonelli, Anna Laura Capriotti, Giorgia La Barbera, Carmela Maria Montone, Susy Piovesana, Aldo Laganà. A Triple Quadrupole and a Hybrid Quadrupole Orbitrap Mass Spectrometer in Comparison for Polyphenol Quantitation. Journal of Agricultural and Food Chemistry. 2019; 67 (17):4885-4896.
Chicago/Turabian StyleChiara Cavaliere; Michela Antonelli; Anna Laura Capriotti; Giorgia La Barbera; Carmela Maria Montone; Susy Piovesana; Aldo Laganà. 2019. "A Triple Quadrupole and a Hybrid Quadrupole Orbitrap Mass Spectrometer in Comparison for Polyphenol Quantitation." Journal of Agricultural and Food Chemistry 67, no. 17: 4885-4896.
An analytical method for determining seleno‐methionine, methyl‐seleno‐cysteine, and seleno‐cystine in wheat bran was developed and validated. Four different extraction procedures were evaluated to simultaneously extract endogenous free and conjugated seleno‐amino acids in wheat bran in order to select the best extraction protocol in terms of seleno amino acid quantitation. The extracted samples were subjected to a clean‐up by a reversed phase/strong cation exchange solid‐phase extraction and analyzed by chiral hydrophilic interaction liquid chromatography‐tandem mass spectrometry. The optimized extraction protocol was employed to validate the methodology. Process efficiency ranged from 58 to 112% and trueness from 73 to 98%. Limit of detection and limit of quantification were lower than 1 ng/g. Four wheat bran samples were analyzed for both total Se and single seleno‐amino acids determination. The results showed that Se‐ seleno‐methyl‐lselenocysteine was the major seleno‐amino acid in wheat bran while seleno‐methionine and seleno‐cysteine were both minor species.
Carmela Maria Montone; Michela Antonelli; Anna Laura Capriotti; Chiara Cavaliere; Giorgia La Barbera; Susy Piovesana; Aldo Laganà. Investigation of free and conjugated seleno‐amino acids in wheat bran by hydrophilic interaction liquid chromatography with tandem mass spectrometry. Journal of Separation Science 2019, 42, 1938 -1947.
AMA StyleCarmela Maria Montone, Michela Antonelli, Anna Laura Capriotti, Chiara Cavaliere, Giorgia La Barbera, Susy Piovesana, Aldo Laganà. Investigation of free and conjugated seleno‐amino acids in wheat bran by hydrophilic interaction liquid chromatography with tandem mass spectrometry. Journal of Separation Science. 2019; 42 (10):1938-1947.
Chicago/Turabian StyleCarmela Maria Montone; Michela Antonelli; Anna Laura Capriotti; Chiara Cavaliere; Giorgia La Barbera; Susy Piovesana; Aldo Laganà. 2019. "Investigation of free and conjugated seleno‐amino acids in wheat bran by hydrophilic interaction liquid chromatography with tandem mass spectrometry." Journal of Separation Science 42, no. 10: 1938-1947.
The combination of an efficient chromatographic separation with post-column addition of a supercharging agent was evaluated for the determination of small peptides. The procedure takes advantage of porous graphitic carbon (PGC) ability in retaining very polar and ionic molecules to overstep the poor retention of small peptides on conventional reversed phase (RP) columns. The method was developed specifically for the most hydrophilic di-, tri- and tetrapeptides, which are not identified in ordinary peptidomics experiments. In addition to retention mechanisms acting on conventional RP, the method exploited the charge induced interactions generated by the charges on the peptides with the polarizable surface of PGC. This results in efficient retention of very short and highly polar peptides using classical RP mobile phases. The effects of varying mobile phase composition (organic solvent and ion-pairing additives) as well as column temperature have been thoroughly investigated using short peptide standards. Under optimized conditions (water and acetonitrile/tetrahydrofuran 99:1 (v/v), both with 0.15% trifluoroacetic acid, as phase A and B, respectively, 0.5 mL min-1 flowrate at 50 °C) the effect of post-column addition of 3-nitrobenzylic alcohol was also investigated allowing effective coupling of the chromatographic system with high resolution mass spectrometry. Finally, an untargeted approach for peptide identification was pursued, based on precursor identification in database with all possible combinations of the 20 natural amino acids and fragmentation spectra matching to in silico generated spectra. The method was then applied to investigation of the short endogenous peptides in in human serum from healthy individuals resulting in the identification of 30 short peptides.
Susy Piovesana; Carmela Maria Montone; Chiara Cavaliere; Carlo Crescenzi; Giorgia La Barbera; Aldo Laganà; Anna Laura Capriotti. Sensitive untargeted identification of short hydrophilic peptides by high performance liquid chromatography on porous graphitic carbon coupled to high resolution mass spectrometry. Journal of Chromatography A 2018, 1590, 73 -79.
AMA StyleSusy Piovesana, Carmela Maria Montone, Chiara Cavaliere, Carlo Crescenzi, Giorgia La Barbera, Aldo Laganà, Anna Laura Capriotti. Sensitive untargeted identification of short hydrophilic peptides by high performance liquid chromatography on porous graphitic carbon coupled to high resolution mass spectrometry. Journal of Chromatography A. 2018; 1590 ():73-79.
Chicago/Turabian StyleSusy Piovesana; Carmela Maria Montone; Chiara Cavaliere; Carlo Crescenzi; Giorgia La Barbera; Aldo Laganà; Anna Laura Capriotti. 2018. "Sensitive untargeted identification of short hydrophilic peptides by high performance liquid chromatography on porous graphitic carbon coupled to high resolution mass spectrometry." Journal of Chromatography A 1590, no. : 73-79.
Nowadays, there is an increasing attention for nutraceuticals and, in general, bioactive compounds naturally present in food. Indeed, the possibility of preserving human health and preventing disease (e.g., cardiovascular diseases, cancer etc.) by the intake of healthy food is attractive for both consumers and food industries. In turn, research in this field was also prompted significantly, with the aim of characterizing these bioactive compounds and ascribe to them a specific activity. The bioactive compounds can belong to several chemical classes. However, their chemical diversity and presence in complex matrices, such as food, make it challenging both their isolation and characterization. To tackle this issue, efficient separation systems are needed, which are mainly based on chromatography. In this context, this mini-review aims to provide the reader with an overview of the most relevant and recent approaches for the separation of the most common bioactive compounds in food, in particular polyphenols, phenols, carotenoids, and peptides, by liquid chromatography approaches.
Chiara Cavaliere; Anna Laura Capriotti; Giorgia La Barbera; Carmela Maria Montone; Susy Piovesana; Aldo Laganà. Liquid Chromatographic Strategies for Separation of Bioactive Compounds in Food Matrices. Molecules 2018, 23, 3091 .
AMA StyleChiara Cavaliere, Anna Laura Capriotti, Giorgia La Barbera, Carmela Maria Montone, Susy Piovesana, Aldo Laganà. Liquid Chromatographic Strategies for Separation of Bioactive Compounds in Food Matrices. Molecules. 2018; 23 (12):3091.
Chicago/Turabian StyleChiara Cavaliere; Anna Laura Capriotti; Giorgia La Barbera; Carmela Maria Montone; Susy Piovesana; Aldo Laganà. 2018. "Liquid Chromatographic Strategies for Separation of Bioactive Compounds in Food Matrices." Molecules 23, no. 12: 3091.
Among the organic contaminants that could pass from waste to polyhydroxyalkanoates (PHAs), there are the polycyclic aromatic hydrocarbons (PAHs). For this reason, we have developed a rapid analytical method for the determination of sixteen PAHs in PHAs. PAHs were extracted by n-hexane, after matrix dispersion and crumbling into sand; the extract was purified by solid phase extraction using florisil as adsorbent. Recoveries in the range of 89–101% were obtained for the deuterated analytes, except for the two with the lowest molecular weight. Trueness between 92% and 108% and within-laboratory precision (expressed as relative standard deviation) ≤ 18% were estimated for all the analytes. Gas chromatography/mass spectrometry was used for analyte determination. Method limits of quantification were suitable to assure that PAH presence in PHA biolpolymers is much below the limits set by European law for plastic materials. Indeed, analysis of two different PHA samples showed that contamination is limited to few compounds at non-concerning levels.
Chiara Cavaliere; Carmela Maria Montone; Anna Laura Capriotti; Giorgia La Barbera; Susy Piovesana; Mauro Rotatori; Francesco Valentino; Aldo Laganà. Extraction of polycyclic aromatic hydrocarbons from polyhydroxyalkanoates before gas chromatography/mass spectrometry analysis. Talanta 2018, 188, 671 -675.
AMA StyleChiara Cavaliere, Carmela Maria Montone, Anna Laura Capriotti, Giorgia La Barbera, Susy Piovesana, Mauro Rotatori, Francesco Valentino, Aldo Laganà. Extraction of polycyclic aromatic hydrocarbons from polyhydroxyalkanoates before gas chromatography/mass spectrometry analysis. Talanta. 2018; 188 ():671-675.
Chicago/Turabian StyleChiara Cavaliere; Carmela Maria Montone; Anna Laura Capriotti; Giorgia La Barbera; Susy Piovesana; Mauro Rotatori; Francesco Valentino; Aldo Laganà. 2018. "Extraction of polycyclic aromatic hydrocarbons from polyhydroxyalkanoates before gas chromatography/mass spectrometry analysis." Talanta 188, no. : 671-675.
The work describes the chromatographic separation optimization of polar lipids on Kinetex-EVO, particularly focusing on sulfolipids in spirulina microalgae (Arthrospira platensis). Gradient shape and mobile-phase modifiers (pH and buffer) were tested on lipid standards. Different conditions were evaluated, and resolution, peak capacity, and peak shape were calculated both in negative mode, for sulfolipids and phospholipids, and in positive mode, for glycolipids. A high-confidence lipid identification strategy was also applied. In collaboration with software creators and developers, Lipostar was implemented to improve the identification of phosphoglycerolipids and to allow the identification of glycosylmonoradyl- and glycosyldiradyl-glycerols classes, the last being the main focus of this work. By this approach, an untargeted screening also for searching lipids not yet reported in the literature could be accomplished. The optimized chromatographic conditions and database search were tested for lipid identification first on the standard mixture, then on the polar lipid extract of spirulina microalgae, for which 205 lipids were identified.
Giorgia La Barbera; Michela Antonelli; Chiara Cavaliere; Gabriele Cruciani; Laura Goracci; Carmela Maria Montone; Susy Piovesana; Aldo Laganà; Anna Laura Capriotti. Delving into the Polar Lipidome by Optimized Chromatographic Separation, High-Resolution Mass Spectrometry, and Comprehensive Identification with Lipostar: Microalgae as Case Study. Analytical Chemistry 2018, 90, 12230 -12238.
AMA StyleGiorgia La Barbera, Michela Antonelli, Chiara Cavaliere, Gabriele Cruciani, Laura Goracci, Carmela Maria Montone, Susy Piovesana, Aldo Laganà, Anna Laura Capriotti. Delving into the Polar Lipidome by Optimized Chromatographic Separation, High-Resolution Mass Spectrometry, and Comprehensive Identification with Lipostar: Microalgae as Case Study. Analytical Chemistry. 2018; 90 (20):12230-12238.
Chicago/Turabian StyleGiorgia La Barbera; Michela Antonelli; Chiara Cavaliere; Gabriele Cruciani; Laura Goracci; Carmela Maria Montone; Susy Piovesana; Aldo Laganà; Anna Laura Capriotti. 2018. "Delving into the Polar Lipidome by Optimized Chromatographic Separation, High-Resolution Mass Spectrometry, and Comprehensive Identification with Lipostar: Microalgae as Case Study." Analytical Chemistry 90, no. 20: 12230-12238.
Selenium is an essential micronutrient for humans. In food, selenium can be present in both inorganic and organic forms, the latter mainly being selenomethionine, Se-methyl-selenocysteine, and selenocystine. Selenoamino acid speciation rarely involves the chirality of selenoamino acids. In this work, a 5 cm long CHIROBIOTIC TAG chromatographic column was used for enantioresolution of selenoamino acids (d- and l-selenomethionine, Se-methyl-l-selenocysteine, d-, l- and meso-selenocystine); in the optimized conditions, the complete resolution of the analytes was achieved within 15 min by using a very polar aqueous mobile phase (gradient elution by methanol/acetonitrile/H2O, 45:45:10 (v/v/v) with 10 mmol L–1 of ammonium formate and 0.5% formic acid as the mobile phase A and acetonitrile/H2O, 20:80 (v/v) with 20 mmol L–1 of ammonium formate at apparent pH 4 as the mobile phase B). The affinity of the teicoplanin aglycone was further exploited to devise a preconcentration method for selenoamino acids in oils. In particular, the CHIROBIOTIC TAG precolumn was used to directly concentrate the selenoamino acids after simple dilution of oil samples with dichloromethane. An optimized procedure for selenoamino acid trapping and preconcentration under normal phase conditions was developed. The enrichment procedure also ensured band focusing during the subsequent separation. The target analytes were finally identified and quantified by triple quadrupole selected reaction monitoring. The method allowed obtainment of recovery values up to 73%, with limits of detection between 280 and 750 ng and limits of quantification between 375 and 960 ng for the different selenoamino acids. The method was applied to commercial oil samples, and only l-selenomethionine was detected.
Anna Laura Capriotti; Carmela Maria Montone; Michela Antonelli; Chiara Cavaliere; Francesco Gasparrini; Giorgia LA Barbera; Susy Piovesana; Aldo Laganà. Simultaneous Preconcentration, Identification, and Quantitation of Selenoamino Acids in Oils by Enantioselective High Performance Liquid Chromatography and Mass Spectrometry. Analytical Chemistry 2018, 90, 8326 -8330.
AMA StyleAnna Laura Capriotti, Carmela Maria Montone, Michela Antonelli, Chiara Cavaliere, Francesco Gasparrini, Giorgia LA Barbera, Susy Piovesana, Aldo Laganà. Simultaneous Preconcentration, Identification, and Quantitation of Selenoamino Acids in Oils by Enantioselective High Performance Liquid Chromatography and Mass Spectrometry. Analytical Chemistry. 2018; 90 (14):8326-8330.
Chicago/Turabian StyleAnna Laura Capriotti; Carmela Maria Montone; Michela Antonelli; Chiara Cavaliere; Francesco Gasparrini; Giorgia LA Barbera; Susy Piovesana; Aldo Laganà. 2018. "Simultaneous Preconcentration, Identification, and Quantitation of Selenoamino Acids in Oils by Enantioselective High Performance Liquid Chromatography and Mass Spectrometry." Analytical Chemistry 90, no. 14: 8326-8330.
In the present paper, bioactive peptides from cauliflower by-products (leaves and stems) were investigated. Alcalase® protein hydrolysis time and pH conditions were optimized, then the hydrolysates were fractionated by preparative RP-HPLC into 12 fractions. Each fraction was tested for the ABTS (2,2′-Azino-bis(3-ethylbenzothiazoline-6-sulfonic acid)), and DPPH (2,2-diphenyl-1-picrylhydrazyl) radical scavenging activity and for ACE (angiotensin-converting enzyme) inhibitor activity. The peptides in the most active fractions were identified by peptidomics technologies and screened for bioactivity by the use of bioinformatics. For ACE-inhibitor activity, two peptides were synthetized, APYDPDWYYIR and SKGFTSPLF, which provided an EC50 value of 2.59 μmol L−1 and 15.26 μmol L−1, respectively. For the ABTS radical scavenging activity, SKGFTSPLF and LDDPVFRPL were tested, and provided an EC50 of 10.35 μmol L−1 and 8.29 μmol L−1, respectively. For the DPPH radical scavenging activity, SKGFTSPLF and LRAPPGWTGR were tested and provided an EC50 of 8.2 μmol L−1 and 5.26 μmol L−1, respectively.
Carmela Maria Montone; Anna Laura Capriotti; Chiara Cavaliere; Giorgia La Barbera; Susy Piovesana; Riccardo Zenezini Chiozzi; Aldo Laganà. Characterization of antioxidant and angiotensin-converting enzyme inhibitory peptides derived from cauliflower by-products by multidimensional liquid chromatography and bioinformatics. Journal of Functional Foods 2018, 44, 40 -47.
AMA StyleCarmela Maria Montone, Anna Laura Capriotti, Chiara Cavaliere, Giorgia La Barbera, Susy Piovesana, Riccardo Zenezini Chiozzi, Aldo Laganà. Characterization of antioxidant and angiotensin-converting enzyme inhibitory peptides derived from cauliflower by-products by multidimensional liquid chromatography and bioinformatics. Journal of Functional Foods. 2018; 44 ():40-47.
Chicago/Turabian StyleCarmela Maria Montone; Anna Laura Capriotti; Chiara Cavaliere; Giorgia La Barbera; Susy Piovesana; Riccardo Zenezini Chiozzi; Aldo Laganà. 2018. "Characterization of antioxidant and angiotensin-converting enzyme inhibitory peptides derived from cauliflower by-products by multidimensional liquid chromatography and bioinformatics." Journal of Functional Foods 44, no. : 40-47.
Microalgae are unicellular marine organisms that have promoted complex biochemical pathways to survive in greatly competitive marine environments. They could contain significant amounts of high-quality proteins which, because of their structural diversity, contain a range of yet undiscovered novel bioactive peptides. In this work, a peptidomic platform was developed for the separation and identification of bioactive peptides in protein hydrolysates. In this work, a peptidomic platform was developed for the extraction, separation, and identification of bioactive peptides in protein hydrolysates. Indeed, extraction of proteins from recalcitrant tissues is still a challenge due to their strong cell walls and high levels of non-protein interfering compounds. Therefore, seven different protein extraction protocols, based on mechanical and chemical methods, were tested in order to produce high-quality protein extracts. Proteins obtained by means of the best protocol, consisting of milling the recalcitrant tissue with glass beads, were subjected to enzymatic digestion with Alcalase® and subsequently the hydrolysate was purified by two-dimensional semi-preparative reversed phase liquid chromatography. Fractions were assayed for antioxidant and antihypertensive activities and only the most active ones were finally analyzed by RP nanoHPLC-MS/MS. Around 500 peptide sequences were identified in these fractions. The identified peptides were subjected to an in silico analysis by PeptideRanker algorithm in order to assign a score of bioactivity probability. Twenty-five sequenced peptides were found with potential antioxidant and angiotensin-converting-enzyme-inhibitory activities. Four of these peptides, WPRGYFL, GPDRPKFLGPF, WYGPDRPKFL, SDWDRF, were selected for synthesis and in vitro tested for specific bioactivity, exhibiting good values of antioxidant and ACE-inhibitory activity.
Carmela Maria Montone; Anna Laura Capriotti; Chiara Cavaliere; Giorgia LA Barbera; Susy Piovesana; Riccardo Zenezini Chiozzi; Aldo Laganà. Peptidomic strategy for purification and identification of potential ACE-inhibitory and antioxidant peptides in Tetradesmus obliquus microalgae. Analytical and Bioanalytical Chemistry 2018, 410, 3573 -3586.
AMA StyleCarmela Maria Montone, Anna Laura Capriotti, Chiara Cavaliere, Giorgia LA Barbera, Susy Piovesana, Riccardo Zenezini Chiozzi, Aldo Laganà. Peptidomic strategy for purification and identification of potential ACE-inhibitory and antioxidant peptides in Tetradesmus obliquus microalgae. Analytical and Bioanalytical Chemistry. 2018; 410 (15):3573-3586.
Chicago/Turabian StyleCarmela Maria Montone; Anna Laura Capriotti; Chiara Cavaliere; Giorgia LA Barbera; Susy Piovesana; Riccardo Zenezini Chiozzi; Aldo Laganà. 2018. "Peptidomic strategy for purification and identification of potential ACE-inhibitory and antioxidant peptides in Tetradesmus obliquus microalgae." Analytical and Bioanalytical Chemistry 410, no. 15: 3573-3586.