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Obesity, a risk factor for the development of type 2 diabetes, represents a socio-economic burden for healthcare systems. Consequently multiple studies aiming to facilitate early diagnostic and prevent complications have demonstrated the promising role of phenolic derivatives on diabetes management. In this frame, the present study aimed to establish for the first time the chemical ingredients and to appraise the antioxidant and the enzyme inhibitory properties of Glycyrrhiza foetida aerial parts and roots extracts using methanol, ethyl acetate and chloroform solvents. The phytochemicals were analyzed via (HPLC-MS/MS). In addition, the extracts were tested for inhibitory activities against α-amylase, α-glucosidase, acetylcholinesterase, butyrylcholinesterase, and tyrosinase. The antioxidant capabilities were evaluated using various methods (phospho‑molybdenum, DPPH, ABTS, FRAP, CUPRAC, and metal chelating assays). Notably, twenty-nine secondary metabolites, namely eleven phenolic acids, seventeen flavonoids and a non-phenolic acid have been identified. Delphinidin 3,5-diglucoside, rutin, isoquercitrin, hyperoside, catechin, phloridzin and hesperidin were the major compounds in the aerial parts extracts while trans-cinnamic acid was the dominant compound in roots. Among phenolic acids, vanillic acid was found to be the main constituent in all extracts. The tested extracts were found to yield TPC in amounts ranging from 34.08 to 49.36 mg GAE/g and TFC ranging from 7.01 to 45.74 mg RE/g. G. foetida extracts showed interesting in vitro antioxidant properties. Additionally, all extracts showed a significant anti-tyrosinase activity, with inhibition values ranging between 52.84 and 80.34 mg KAE/g. Thus, G. foetida remains an exceptional matrix for further investigations and application in cosmetics and food additives., Competing Interests: Declaration of competing interest The authors declare no conflict of interest., (Copyright © 2024 Elsevier B.V. All rights reserved.)

A new fast and easy analytical procedure for the simultaneous detection and quantification of 9 anabolic steroids (deslorelin, dexamethasone sodium phosphate, prednisolone, methylprednisolone, stanozolol, boldenone, nandrolone, dexamethasone isonicotinate and altrenogest) in horse urine for doping control have been developed by using the ultra-high-performance liquid chromatography coupled with tandem mass spectrometry technique (UHPLC-MS/MS). A total amount of 400 μl of sample was evaporated, restored and injected in the UHPLC-MS/MS. The proposed method was fully validated showing a recovery higher than 89.12% and a coefficient of variation lower than 6.02%. The correlation coefficients range of the analyzed compound's calibration curves was 0.9955-0.9997, and the limits of detection and quantification were in the range of 0.1 and 0.25 μg/l, respectively., (Copyright © 2019 Elsevier B.V. All rights reserved.)

Polycyclic aromatic hydrocarbons (PAHs) and polychlorinated biphenyls (PCBs) are priority contaminants that bioaccumulate through the food webs and affect the biology of a variety of resident and migratory species, including sea turtles. Few studies have evaluated toxicological biomarkers of exposure to PAHs and PCBs in these animals. The present paper reports the results of an initial field study to quantify the association between plasma concentrations of PAHs/PCBs and whole blood cell expression of gene biomarkers in juvenile loggerhead sea turtles (Caretta caretta) rescued along the Italian coasts of the northern and central areas of the Adriatic Sea. While detectable levels of PAHs were found in all plasma samples examined, only three PCB congeners (PCB52, PCB95, and PCB149) were noted, with detection percentages ranging between 48% and 57%. A significant correlation was found between 3 of the 6 gene biomarkers assessed (HSP60, CYP1A and ERα) and plasma levels of some PAH congeners. In contrast, no significant association between PCB burden and gene expression was observed. The global DNA methylation levels were significantly and positively correlated with the concentrations of most of the PAHs and only one of the PCB congeners (PCB52). The relation between PAH concentration and gene expression in whole blood cells suggests that these genes may respond to environmental contaminant exposure and are promising candidates for the development of biomarkers for monitoring sea turtle exposure to persistent organic pollutants (POPs)., (Copyright © 2017 Elsevier B.V. All rights reserved.)

Recent evidences suggest that the toxicological effects of endocrine disrupting chemicals (EDCs) involve multiple nuclear receptor-mediated pathways, including estrogen receptor (ER) and peroxisome proliferator-activated receptor (PPAR) signaling systems. Thus, our objective in this study was to detect the summated endocrine effects of EDCs with metabolic activity in coastal waters of the central Adriatic Sea by means of a toxicogenomic approach using seabream hepatocytes. Gene expression patterns were also correlated with seawater levels of polychlorinated biphenyls (PCBs) and polycyclic aromatic hydrocarbons (PAHs). We found that seawater extracts taken at certain areas induced gene expression profiles of ERα/vitellogenin, PPARα/Stearoyl-CoA desaturase 1A, cytochrome P4501A (CYP1A) and metallothionein. These increased levels of biomarkers responses correlated with spatial distribution of PAHs/PCBs concentrations observed by chemical analysis in the different study areas. Collectively, our data give a snapshot of the presence of complex EDC mixtures that are able to perturb metabolic signaling in coastal marine waters., (Copyright © 2016 Elsevier Ltd. All rights reserved.)

In order to assess if an extra virgin olive oil (EVOO) can be acknowledged with the health claim related to olive oil polyphenols (Reg. EU n.432/2012), a new method to quantify these species in EVOO, by means of liquid-liquid extraction followed by HPLC-DAD/MS/MS of the hydroalcoholic extract, has been developed and validated. Different extraction procedures, different types of reverse-phase analytical columns (Synergi Polar, Spherisorb ODS2 and Kinetex) and eluents have been tested. The chromatographic column Synergi Polar (250×4.6mm, 4μm), never used before in this kind of application, provided the best results, with water and methanol/isopropanol (9/1) as eluents. The method allows the quantification of the phenolic alcohols tyrosol and hydroxytyrosol, the phenolic acids vanillic, p-coumaric and ferulic acids, secoiridoids derivatives, the lignans, pinoresinol and acetoxypinoresinol and the flavonoids luteolin and apigenin. The new method has been applied to 20 commercial EVOOs belonging to two different price range categories (3.78-5.80 euros/L and 9.5-25.80 euros/L) and 5 olive oils. The obtained results highlight that acetoxypinoresinol, ferulic acid, vanillic acid and the total non secoiridoid phenolic substances resulted to be significantly higher in HEVOOs than in LEVOOs (P=0.0026, 0.0217, 0.0092, 0.0003 respectively). For most of the samples analysed there is excellent agreement between the results obtained by applying the HPLC method adopted by the International Olive Council and the results obtained by applying the presented HPLC method. Results obtained by HPLC methods have been also compared with the ones obtained by the colorimetric Folin-Ciocalteu method., (Copyright © 2016 Elsevier B.V. All rights reserved.)

Aim: Celiac disease (CD) is a systemic immune-mediated enteropathy sustained by gluten ingestion in genetically susceptible subjects. The European Society for Pediatric Gastroenterology, Hepatology and Nutrition (ESPGHAN) has recently revised the diagnostic criteria, emphasizing the crucial role of serological testing in the diagnosis of this condition. This study was hence aimed to evaluate a new chemiluminescence assay for measuring anti-transglutaminase (tTG) and anti-endomysium (EMA) antibodies in a general population of unselected outpatients., Materials and Methods: The IgA and IgG anti-tissue transglutaminase (tTG) antibodies (Quanta Flash® IgA and Quanta Flash® IgG tTG, Inova Diagnostics, San Diego, CA, USA) were measured with the fully-automated BIO-FLASH® analyzer (Inova Diagnostics) in serum samples of 727 consecutive patients without a diagnosis of CD. Data were compared with those of anti-endomysium antibody (EmA) obtained in the same population., Results: A total of 96.4% samples display a negative concordance (anti-tTG negative and EMA negative), O% were positive for EMA and negative for anti-tTG IgA and IgG, 3.6% were both positive for tTG IgA and EMA, whereas 0.6% displayed discordant results (positive for anti-tTG and negative for EMA). The concordance (99%) and inter-rater agreement (Kappa Statistics, 0.943; p<0.001) between anti-tTG IgA and EmA antibodies were excellent, with sensitivity and specificity of 99% and 100%, respectively., Conclusion: The results of this study show that Quanta Flash® IgA assay alone may be regarded as a reliable approach for screening of CD, with no need to perform EMA detection., (Copyright © 2016 Elsevier B.V. All rights reserved.)

In the present work we carried out a phytochemical and biological investigation on three Hypericum species, i.e. Hypericum reflexum, Hypericum canariense and Hypericum grandifolium, from the Canary Islands where they are traditionally used as diuretic, wound healing, vermifuge, sedative and antidepressive agents. The polar extracts of the top flowering aerial parts, prepared by Soxhlet apparatus using a methanol-acetone (1:1) extracting mixture, were analyzed by HPLC-DAD and HPLC-MS for the content of eight biomarkers such as hypericin, hyperforin, chlorogenic acid, rutin, hyperoside, isoquercitrin, quercitrin and quercetin, whereas the hydrodistilled essential oils were analyzed by GC-FID and GC-MS. The three Hypericum species had different results in both polar and volatile constituents, H. reflexum being the only one endowed with a small amount of naphtodianthrones (hypericin and pseudohypericin), and containing high levels of chlorogenic acid, rutin and volatile mono- and sesquiterpenes. After chemical characterization, all products were in vitro biologically assayed for antiproliferative activity on human tumor cell lines by MTT assay, for antioxidant potential by DPPH, ABTS and FRAP assays, and for antimicrobial activity by the agar disc diffusion and microdilution methods. Results revealed interesting bioactivities and differences between polar extracts and essential oils, with the former being endowed with significant antioxidant activity and the latter with comparable inhibition effects on the tumor cells (A375, MDA-MB 231 and HCT 116) to that of cisplatin., (Copyright © 2014 Elsevier B.V. All rights reserved.)

In this work, we present for the first time a rapid and robust UHPLC-MS/MS method for analyzing taurine, GlcLA and GlcA in energy drinks simultaneously and without derivatization. The separation of three analytes was achieved using a Kinetex Hilic analytical column (100 mm × 4.6 mm i.d.) and a mobile phase formed by water (A) and acetonitrile (B) both with formic acid 0.1% at a flow rate of 0.8 ml min(-1) with isocratic elution in 3.5 min. Calibration curves were calculated using the method of standard addition in a concentration range from 2 to 6 mg/100 ml for taurine (R(2)>0.987), from 0.4 to 1.2 mg/100 ml for GlcLa (R(2)>0.997), and from 0.2 to 0.6 mg/100 ml for GlcA acid (R(2)>0.998). The validated method was applied to the analysis of nine commercial energy drinks. The level of taurine found ranged from 0.01 to 0.45 g/100 ml, and it matched with that reported in the labels of the analyzed energy drink samples., (Copyright © 2014 Elsevier B.V. All rights reserved.)

Coumarin occurs in many plants used as flavoring and is known to possess hepatotoxic effects. Despite in the EFSA 'Compendium of botanicals containing toxic substances' coumarin is reported to be present in Melittis melissophyllum (bastard balm), a plant traditionally used as beverage in Italy and Serbia, to the best of our knowledge quantitative data has never been reported. Thus, the amount of coumarin in bastard balm leaves and its variation during the annual phenological cycle were determined. The subsp. melissophyllum resulted to contain high levels of coumarin (14,392 mg/kg), mainly in the early stages of the plant cycle, suggesting prudence in its use as beverage. Furthermore, coumarin was found to be useful as marker compound to differentiate the bastard balm subspecies occurring in Italy, since the subsp. albida contained a much lower content of this molecule (19-34 mg/kg)., (Copyright © 2011 Elsevier B.V. All rights reserved.)

A new analytical method that uses high performance liquid chromatography-diode array detector (HPLC-DAD) was developed for the analysis of 14 benzimidazoles residues, including metabolites, in bovine liver. Samples were extracted using two different extraction procedures: with phosphate buffer after enzymatic hydrolysis (method A) or using organic solvent, i.e. acetonitrile (method B). Then, samples were purified on a strong cation exchange (SCX) cartridge and analyzed in HPLC/DAD. The recovery percentages, obtained spiking the matrix (liver) at concentrations of 500 and 100 microg kg(-1) with a standard mixture of benzimidazoles, were in the range 6-101% and 80-102% for methods A and B, respectively. The repeatability of the methods was assessed in all cases by the % of correlation value (CV) that was lower than 19%. The limits of quantification (LOQs) in the matrix for methods A and B were in the range 40-60 and 20-50 microg kg(-1), respectively. The best of the two methods, method B, was used for the analysis of 10 bovine liver samples., (Copyright (c) 2010 Elsevier B.V. All rights reserved.)

A new analytical method, using gas chromatography-mass spectrometry (GC/MS) and liquid chromatography-mass spectrometry (LC/MS) techniques, was developed for the determination in packaged food beverages of five ink photoinitiator residues: 2-isopropylthioxanthone (ITX), benzophenone, 2-ethylhexyl-4-dimethylaminobenzoate (EHDAB), 1-hydroxycyclohexyl-1-phenyl ketone (IRGACURE 184) and ethyl-4-dimethylaminobenzoate (EDAB). Samples were extracted from selected beverages (milk, fruit juices and wine) and relative packagings, using n-hexane and dichloromethane, respectively, purified on solid-phase extraction (SPE) silica gel cartridges, and then analyzed in GC/MS and LC/MS. The recovery percentages, obtained spiking the beverage samples at concentrations of 4 and 10 microgl(-1) with a standard mixture of photoinitiators, were in the range 42-108% (milk), 50-84% (wine), and 48-109% (fruit juices). The repeatability of the method was assessed in all cases by the % of correlation value, that was lower than 19%. The lowest limits of detection (LODs) and limits of quantification (LOQs), obtained using GC/MS, were in the range 0.2-1 and 1-5 microgl(-1), respectively. The method was applied to the analysis of forty packaged food beverages (milk, fruit juices and wine samples). The most significant contamination was that of benzophenone, found in all samples in a concentration range of 5-217mugl(-1). Its presence was confirmed by an LC/Atmospheric-Pressure PhotoIonization (APPI)/MS/MS analysis. The photoinitiator (EHDAB) was found in eleven out of forty beverages in a concentration range of 0.13-0.8 microgl(-1). Less important was the ITX contamination, found in three out of forty samples in a range 0.2-0.24 microgl(-1). The work proposes a new method to analyze ink photoinitiator residues in polycoupled carton packaging and in contained food beverages.