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Article ; Online: Analytical methods employed in the identification and quantification of per- and polyfluoroalkyl substances in human matrices - A scoping review.

Comito, Rossana / Porru, Emanuele / Violante, Francesco Saverio

2023 Volume 345, Page(s) 140433

Abstract: Persistent organic pollutants (POPs) represent a possible hazard for the ecosystems, with adverse outcomes on wildlife and humans. POPs have always received interest from the scientific community, and they have also been subject to legal restrictions ... ...

Abstract	Persistent organic pollutants (POPs) represent a possible hazard for the ecosystems, with adverse outcomes on wildlife and humans. POPs have always received interest from the scientific community, and they have also been subject to legal restrictions worldwide on their application and commercialization. Among the broad spectrum of POPs, per- and polyfluoroalkyl substances (PFASs) are considered emerging contaminants due to their potential effect on the ecosystem and human health. These contaminants are widely employed in countless applications, from surfactants and building materials to food packaging. On the other hand, their chemical structure gives them the ability to interact with the environment, causing possible toxic effects for humans and environment. Human biomonitoring is a necessary instrument to indagate the impact of PFASs on human health: in recent years several studies have found detectable levels of PFASs in several biological matrices in humans (blood, hair, nails, and urine). Here, we review the most recent scientific literature concerning analytical methods employed in the identification and quantification of PFASs focusing on biological matrices. It has been noted that liquid chromatography coupled with mass spectrometry is the main analytical instrumentation employed, while blood and/or serum samples are the main employed human matrices whereas the use of non-invasive matrices is still at the beginning. Various issues directly related to human metabolism of PFASs and the effective amount of PFAS absorbed from the environment still need to be investigated.
MeSH term(s)	Humans ; Ecosystem ; Chromatography, Liquid ; Mass Spectrometry ; Environmental Pollutants/analysis ; Fluorocarbons/analysis
Chemical Substances	Environmental Pollutants ; Fluorocarbons
Language	English
Publishing date	2023-10-11
Publishing country	England
Document type	Journal Article ; Review
ZDB-ID	120089-6
ISSN	1879-1298 ; 0045-6535 ; 0366-7111
ISSN (online)	1879-1298
ISSN	0045-6535 ; 0366-7111
DOI	10.1016/j.chemosphere.2023.140433
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Article ; Online: Analysis of fecal bile acids and metabolites by high resolution mass spectrometry in farm animals and correlation with microbiota.

Porru, Emanuele / Scicchitano, Daniel / Interino, Nicolò / Tavella, Teresa / Candela, Marco / Roda, Aldo / Fiori, Jessica

Scientific reports

2022 Volume 12, Issue 1, Page(s) 2866

Abstract: There is a growing interest in the named "acidic sterolbiome" and in the genetic potential of the gut microbiome (GM) to modify bile acid (BA) structure. Indeed, the qualitative composition of BAs in feces correlates with the bowel microorganisms and ... ...

Abstract	There is a growing interest in the named "acidic sterolbiome" and in the genetic potential of the gut microbiome (GM) to modify bile acid (BA) structure. Indeed, the qualitative composition of BAs in feces correlates with the bowel microorganisms and their collective genetic material. GM is responsible for the production of BA metabolites, such as secondary and oxo-BAs. The specific BA profiles, as microbiome-host co-metabolic products, could be useful to investigate the GM-host interaction in animals under physiological conditions, as well as in specific diseases. In this context, we developed and validated an ultra-performance liquid chromatography-quadrupole time-of-flight mass spectrometry method for the simultaneous analysis of up to 21 oxo-BAs and their 9 metabolic precursors. Chromatographic separation was achieved in 7 min with adequate analytical performance in terms of selectivity, sensitivity (LOQ from 0.05 to 0.1 µg/mL), accuracy (bias% < 5%), precision (CV% < 5%) and matrix effect (ME% < 10%). A fast solvent extraction protocol has been fine-tuned, achieving recoveries > 90%. In parallel, the gut microbiota assessment in farming animals was evaluated by 16S rRNA next-generation sequencing, and the correlation with the BA composition was performed by multivariate analysis, allowing to reconstruct species-specific associations between the BA profile and specific GM components.
MeSH term(s)	Animals ; Animals, Domestic/metabolism ; Animals, Domestic/microbiology ; Bile Acids and Salts/analysis ; Bile Acids and Salts/metabolism ; Chromatography, Liquid/methods ; Feces/chemistry ; Gastrointestinal Microbiome/genetics ; High-Throughput Nucleotide Sequencing ; Host Microbial Interactions ; Mass Spectrometry/methods ; RNA, Bacterial/genetics ; Sensitivity and Specificity ; Species Specificity
Chemical Substances	Bile Acids and Salts ; RNA, Bacterial
Language	English
Publishing date	2022-02-21
Publishing country	England
Document type	Journal Article ; Research Support, Non-U.S. Gov't
ZDB-ID	2615211-3
ISSN	2045-2322 ; 2045-2322
ISSN (online)	2045-2322
ISSN	2045-2322
DOI	10.1038/s41598-022-06692-9
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Article: Metabolic Bile Acid Profile Impairments in Dogs Affected by Chronic Inflammatory Enteropathy.

Comito, Rossana / Porru, Emanuele / Interino, Nicolò / Conti, Matteo / Terragni, Rossella / Gotti, Roberto / Candela, Marco / Simoni, Patrizia / Roda, Aldo / Fiori, Jessica

Metabolites

2023 Volume 13, Issue 9

Abstract: Bile acids (BAs), endogenous acidic steroids synthetized from cholesterol in the liver, play a key role in the gut-liver axis physiopathology, including in hepatotoxicity, intestinal inflammatory processes, and cholesterol homeostasis. Faecal Oxo-BAs, ... ...

Abstract	Bile acids (BAs), endogenous acidic steroids synthetized from cholesterol in the liver, play a key role in the gut-liver axis physiopathology, including in hepatotoxicity, intestinal inflammatory processes, and cholesterol homeostasis. Faecal Oxo-BAs, relatively stable intermediates of oxidation/epimerization reactions of the BA hydroxyls, could be relevant to investigating the crosstalk in the liver-gut axis and the relationship between diseases and alterations in microbiota composition. A paucity of information currently exists on faecal BA profiles in dogs with and without chronic inflammatory enteropathy (CIE). Comprehensive assessment of 31 molecules among faecal BAs and related microbiota metabolites was conducted with high-performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS). Odds ratios (ORs) for associations of BAs with CIE were estimated using logistic regression. Principal component analysis was performed to find differences between the control and pathological dogs. Higher levels of primary BAs and muricholic acids, and lower levels of secondary BAs were found in pathological dogs. Higher concentrations in faecal oxo-metabolites were associated with the absence of CIE (OR < 1). This study shows a marked difference in faecal BA profiles between dogs with and without CIE. Further research will be needed to better understand the role of oxo-BAs and muricholic acids in CIE dogs.
Language	English
Publishing date	2023-08-30
Publishing country	Switzerland
Document type	Journal Article
ZDB-ID	2662251-8
ISSN	2218-1989
ISSN	2218-1989
DOI	10.3390/metabo13090980
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Article ; Online: Extraction method for the multiresidue analysis of legacy and emerging pollutants in marine mussels from the Adriatic Sea

Interino, Nicolò / Comito, Rossana / Simoni, Patrizia / Franzellitti, Silvia / Palladino, Giorgia / Rampelli, Simone / Mosendz, Anastasiia / Gotti, Roberto / Roda, A. / Candela, Marco / Porru, Emanuele / Fiori, Jessica

Food Chemistry. 2023 May 26, p.136453-

2023 , Page(s) 136453–

Abstract: The release of hazardous chemicals into aquatic environments has long been a known problem, but its full impact has only recently been realized. This study presents a validated liquid chromatography–mass spectrometry (HPLC–MS/MS) method for detecting ... ...

Abstract	The release of hazardous chemicals into aquatic environments has long been a known problem, but its full impact has only recently been realized. This study presents a validated liquid chromatography–mass spectrometry (HPLC–MS/MS) method for detecting pharmaceutical and pesticide residues in mussels (Mytilus galloprovincialis). An innovative MS-compatible extraction method was developed and validated, demonstrating successful recovery rates for analytes at three different concentration levels (25-95%). The method detected the target analytes at ng/g concentrations with high accuracy (-7% to 11%) and low relative standard deviation (<10%) for both intra-day and inter-day analyses. After validation, the method was applied to mussel samples collected from a commercial farm near Senigallia, Adriatic Sea, detecting different contaminants in the range of 2-40 ng/g (dry weight). The study provides a valuable tool for investigating the potential threats posed by diverse contaminant classes with high annual tonnage, including analytes with known persistence and/or illegal status.
Keywords	Mytilus galloprovincialis ; chemical species ; commercial farms ; food chemistry ; liquid chromatography ; mass spectrometry ; multiresidue analysis ; mussels ; pesticides ; standard deviation ; Adriatic Sea ; Analytical method validation ; LC-MS ; Bivalve mollusks ; Pharmaceuticals ; Food pollution
Language	English
Dates of publication	2023-0526
Publishing place	Elsevier Ltd
Document type	Article ; Online
Note	Pre-press version
ZDB-ID	243123-3
ISSN	1873-7072 ; 0308-8146
ISSN (online)	1873-7072
ISSN	0308-8146
DOI	10.1016/j.foodchem.2023.136453
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Article: Intestinal FXR Activation via Transgenic Chimera or Chemical Agonism Prevents Colitis-Associated and Genetically-Induced Colon Cancer.

Cariello, Marica / Zerlotin, Roberta / Pasculli, Emanuela / Piccinin, Elena / Peres, Claudia / Porru, Emanuele / Roda, Aldo / Gadaleta, Raffaella Maria / Moschetta, Antonio

Cancers

2022 Volume 14, Issue 13

Abstract: The Farnesoid X Receptor (FXR) is the master regulator of Bile Acids (BA) homeostasis orchestrating their synthesis, transport and metabolism. Disruption of BA regulation has been linked to gut-liver axis diseases such as colorectal cancer (CRC). In this ...

Abstract	The Farnesoid X Receptor (FXR) is the master regulator of Bile Acids (BA) homeostasis orchestrating their synthesis, transport and metabolism. Disruption of BA regulation has been linked to gut-liver axis diseases such as colorectal cancer (CRC). In this study, firstly we examined the role of constitutive activation of intestinal FXR in CRC; then we pre-clinically investigated the therapeutic potential of a diet enriched with a synthetic FXR agonist in two models of CRC (chemically-induced and genetic models). We demonstrated that mice with intestinal constitutive FXR activation are protected from AOM/DSS-induced CRC with a significant reduction of tumor number compared to controls. Furthermore, we evaluated the role of chemical FXR agonism in a DSS model of colitis in wild type (WT) and FXR
Language	English
Publishing date	2022-06-23
Publishing country	Switzerland
Document type	Journal Article
ZDB-ID	2527080-1
ISSN	2072-6694
ISSN	2072-6694
DOI	10.3390/cancers14133081
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Article ; Online: Seasonal dynamics of the microbiome-host response to pharmaceuticals and pesticides in Mytilus galloprovincialis farmed in the Northwestern Adriatic Sea.

Palladino, Giorgia / Rampelli, Simone / Scicchitano, Daniel / Nanetti, Enrico / Iuffrida, Letizia / Wathsala, Rajapaksha Haddokara Gedara Rasika / Interino, Nicolò / Marini, Mauro / Porru, Emanuele / Turroni, Silvia / Fiori, Jessica / Franzellitti, Silvia / Candela, Marco

The Science of the total environment

2023 Volume 887, Page(s) 163948

Abstract: Marine mussels, especially Mytilus galloprovincialis, are well-established sentinel species, being naturally resistant to the exposure to multiple xenobiotics of natural and anthropogenic origin. Even if the response to multiple xenobiotic exposure is ... ...

Abstract	Marine mussels, especially Mytilus galloprovincialis, are well-established sentinel species, being naturally resistant to the exposure to multiple xenobiotics of natural and anthropogenic origin. Even if the response to multiple xenobiotic exposure is well known at the host level, the role of the mussel-associated microbiome in the animal response to environmental pollution is poorly explored, despite its potential in xenobiotic detoxification and its important role in host development, protection, and adaptation. Here, we characterized the microbiome-host integrative response of M. galloprovincialis in a real-world setting, involving exposure to a complex pattern of emerging pollutants, as occurs in the Northwestern Adriatic Sea. A total of 387 mussel individuals from 3 commercial farms, spanning about 200 km along the Northwestern Adriatic coast, and in 3 different seasons, were collected. Multiresidue analysis (for quantitative xenobiotic determination), transcriptomics (for host physiological response), and metagenomics (for host-associated microbial taxonomical and functional features) analyses were performed on the digestive glands. According to our findings, M. galloprovincialis responds to the presence of the complex pattern of multiple emerging pollutants - including the antibiotics sulfamethoxazole, erythromycin, and tetracycline, the herbicides atrazine and metolachlor, and the insecticide N,N-diethyl-m-toluamide - integrating host defense mechanisms, e.g., through upregulation of transcripts involved in animal metabolic activity, and microbiome-mediated detoxification functions, including microbial functionalities involved in multidrug or tetracycline resistance. Overall, our data highlight the importance of the mussel-associated microbiome as a strategic player for the orchestration of resistance to the multixenobiotic exposure at the holobiont level, providing strategic functionalities for the detoxification of multiple xenobiotic substances, as occurring in real world exposure settings. Complementing the host with microbiome-dependent xenobiotic degradative and resistance genes, the M. galloprovincialis digestive gland associated microbiome can have an important role in the detoxification of emerging pollutants in a context of high anthropogenic pressure, supporting the relevance of mussel systems as potential animal-based bioremediation tool.
MeSH term(s)	Animals ; Mytilus/metabolism ; Seasons ; Pesticides/analysis ; Xenobiotics/metabolism ; Microbiota ; Water Pollutants, Chemical/analysis
Chemical Substances	Pesticides ; Xenobiotics ; Water Pollutants, Chemical
Language	English
Publishing date	2023-05-05
Publishing country	Netherlands
Document type	Journal Article
ZDB-ID	121506-1
ISSN	1879-1026 ; 0048-9697
ISSN (online)	1879-1026
ISSN	0048-9697
DOI	10.1016/j.scitotenv.2023.163948
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Article ; Online: Extraction method for the multiresidue analysis of legacy and emerging pollutants in marine mussels from the Adriatic Sea.

Interino, Nicolò / Comito, Rossana / Simoni, Patrizia / Franzellitti, Silvia / Palladino, Giorgia / Rampelli, Simone / Mosendz, Anastasiia / Gotti, Roberto / Roda, Aldo / Candela, Marco / Porru, Emanuele / Fiori, Jessica

Food chemistry

2023 Volume 425, Page(s) 136453

Abstract: The release of hazardous chemicals into aquatic environments has long been a known problem, but its full impact has only recently been realized. This study presents a validated liquid chromatography-mass spectrometry (HPLC-MS/MS) method for detecting ... ...

Abstract	The release of hazardous chemicals into aquatic environments has long been a known problem, but its full impact has only recently been realized. This study presents a validated liquid chromatography-mass spectrometry (HPLC-MS/MS) method for detecting pharmaceutical and pesticide residues in mussels (Mytilus galloprovincialis). An innovative MS-compatible extraction method was developed and validated, demonstrating successful recovery rates for analytes at three different concentration levels (25-95%). The method detected the target analytes at ng/g concentrations with high accuracy (-7% to 11%) and low relative standard deviation (<10%) for both intra-day and inter-day analyses. After validation, the method was applied to mussel samples collected from a commercial farm near Senigallia, Adriatic Sea, detecting different contaminants in the range of 2-40 ng/g (dry weight). The study provides a valuable tool for investigating the potential threats posed by diverse contaminant classes with high annual tonnage, including analytes with known persistence and/or illegal status.
MeSH term(s)	Animals ; Tandem Mass Spectrometry ; Environmental Pollutants/analysis ; Water Pollutants, Chemical/analysis ; Mytilus/chemistry ; Hazardous Substances
Chemical Substances	Environmental Pollutants ; Water Pollutants, Chemical ; Hazardous Substances
Language	English
Publishing date	2023-05-26
Publishing country	England
Document type	Journal Article
ZDB-ID	243123-3
ISSN	1873-7072 ; 0308-8146
ISSN (online)	1873-7072
ISSN	0308-8146
DOI	10.1016/j.foodchem.2023.136453
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Article ; Online: Bile acids and oxo-metabolites as markers of human faecal input in the ancient Pompeii ruins.

Porru, Emanuele / Giorgi, Enrico / Turroni, Silvia / Helg, Riccardo / Silani, Michele / Candela, Marco / Fiori, Jessica / Roda, Aldo

Scientific reports

2021 Volume 11, Issue 1, Page(s) 3650

Abstract: Small organic molecules, lipids, proteins, and DNA fragments can remain stable over centuries. Powerful and sensitive chemical analysis can therefore be used to characterize ancient remains for classical archaeological studies. This bio-ecological ... ...

Abstract	Small organic molecules, lipids, proteins, and DNA fragments can remain stable over centuries. Powerful and sensitive chemical analysis can therefore be used to characterize ancient remains for classical archaeological studies. This bio-ecological dimension of archaeology can contribute knowledge about several aspects of ancient life, including social organization, daily habits, nutrition, and food storage. Faecal remains (i.e. coprolites) are particularly interesting in this regard, with scientists seeking to identify new faecal markers. Here, we report the analysis of faecal samples from modern-day humans and faecal samples from a discharge pit on the site of the ruins of ancient Pompeii. We propose that bile acids and their gut microbiota oxo-metabolites are the most specific steroid markers for detecting faecal inputs. This is due to their extreme chemical stability and their exclusive occurrence in vertebrate faeces, compared to other ubiquitous sterols and steroids.
MeSH term(s)	Archaeology ; Bile Acids and Salts/chemistry ; Bile Acids and Salts/isolation & purification ; Body Remains/chemistry ; DNA/chemistry ; DNA, Ancient/chemistry ; Feces/chemistry ; Humans ; Lipids/chemistry ; Metabolome/genetics ; Proteins/chemistry
Chemical Substances	Bile Acids and Salts ; DNA, Ancient ; Lipids ; Proteins ; DNA (9007-49-2)
Language	English
Publishing date	2021-02-11
Publishing country	England
Document type	Journal Article ; Research Support, Non-U.S. Gov't
ZDB-ID	2615211-3
ISSN	2045-2322 ; 2045-2322
ISSN (online)	2045-2322
ISSN	2045-2322
DOI	10.1038/s41598-021-82831-y
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Article ; Online: Grape Pomace for Topical Application: Green NaDES Sustainable Extraction, Skin Permeation Studies, Antioxidant and Anti-Inflammatory Activities Characterization in 3D Human Keratinocytes.

Punzo, Angela / Porru, Emanuele / Silla, Alessia / Simoni, Patrizia / Galletti, Paola / Roda, Aldo / Tagliavini, Emilio / Samorì, Chiara / Caliceti, Cristiana

Biomolecules

2021 Volume 11, Issue 8

Abstract: Food waste is a global problem due to its environmental and economic impact, so there is great demand for the exploitation of new functional applications. The winemaking process leads to an incomplete extraction of high-value compounds, leaving the ... ...

Abstract	Food waste is a global problem due to its environmental and economic impact, so there is great demand for the exploitation of new functional applications. The winemaking process leads to an incomplete extraction of high-value compounds, leaving the pomace still rich in polyphenols. This study was aimed at optimising and validating sustainable routes toward the extraction and further valorisation of these polyphenols, particularly for cosmeceutical applications. New formulations based on red grape pomace polyphenols and natural deep eutectic solvents (NaDESs) were here investigated, namely betaine combined with citric acid (BET-CA), urea (BET-U) and ethylene glycol (BET-EG), in which DESs were used both as extracting and carrying agents for polyphenols. The flavonoid profile determined by HPLC-MS/MS analysis showed similar malvidin content (51-56 μg mL
MeSH term(s)	Anti-Inflammatory Agents/pharmacology ; Antioxidants/pharmacology ; Cosmetics/chemistry ; HaCaT Cells ; Humans ; Oxidative Stress/drug effects ; Plant Extracts/pharmacology ; Polyphenols/pharmacology ; Refuse Disposal/methods ; Vitis/metabolism
Chemical Substances	Anti-Inflammatory Agents ; Antioxidants ; Cosmetics ; Plant Extracts ; Polyphenols
Language	English
Publishing date	2021-08-10
Publishing country	Switzerland
Document type	Journal Article ; Research Support, Non-U.S. Gov't
ZDB-ID	2701262-1
ISSN	2218-273X ; 2218-273X
ISSN (online)	2218-273X
ISSN	2218-273X
DOI	10.3390/biom11081181
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Article: Combined analytical approaches to define biodistribution and biological activity of semi-synthetic berberrubine, the active metabolite of natural berberine

Porru, Emanuele / Aldo Roda / Cristiana Caliceti / Donato Calabria / Marinella Roberti / Placido Franco / Silvia Spinozzi

Analytical and bioanalytical chemistry. 2018 June, v. 410, no. 15

2018

Abstract: Berberine (BBR) is a natural alkaloid obtained from Berberis species plants, known for its protective effects against several diseases. Among the primary BBR metabolites, berberrubine (M1) showed the highest plasma concentration but few and conflicting ... ...

Abstract	Berberine (BBR) is a natural alkaloid obtained from Berberis species plants, known for its protective effects against several diseases. Among the primary BBR metabolites, berberrubine (M1) showed the highest plasma concentration but few and conflicting data are available regarding its concentration in biological fluids related to its new potential activity on vascular cells. A combined analytical approach was applied to study biodistribution of M1 in comparison with BBR. The optimization of sample clean-up combined with a fully validated HPLC-ESI-MS/MS tailored for M1 allows sufficient detectability and accuracy to be reached in the different studied organs even when administered at low dose, comparable to that assumed by human. A predictive human vascular endothelial cell-based assay to measure intracellular xanthine oxidase has been developed and applied to study unexplored activities of M1 alongside other common activities. Results showed that oral M1 treatment exhibits higher plasma levels than BBR, reaching maximum concentration 400-fold higher than BBR (204 vs 0.5 ng/mL); moreover, M1 exhibits higher concentrations than BBR also in all the biological compartments analyzed. Noteworthy, the two compounds follow two different excretion routes: M1 through urine, while BBR through feces. In vitro studies demonstrated that M1 inhibited intracellular xanthine oxidase activity, one of the major sources of reactive oxygen species in vasculature, with an IC50 = 9.90 ± 0.01 μg/mL and reduced the expression of the inflammatory marker ICAM-1. These peculiar characteristics allow new perspectives to be opened up for the direct use of M1 instead of BBR in endothelial dysfunction treatment.
Keywords	analytical methods ; berberine ; Berberis ; enzyme activity ; excretion ; feces ; humans ; in vitro studies ; inhibitory concentration 50 ; intercellular adhesion molecule-1 ; metabolites ; protective effect ; urine ; xanthine oxidase
Language	English
Dates of publication	2018-06
Size	p. 3533-3545.
Publishing place	Springer Berlin Heidelberg
Document type	Article
ISSN	1618-2642
DOI	10.1007/s00216-018-0884-2
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