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1.
Molecules ; 27(14)2022 Jul 12.
Article in English | MEDLINE | ID: mdl-35889326

ABSTRACT

Tandem mass spectrometry is proposed to check lipid oxidation, a free radical-mediated phenomenon which effects oxidative deterioration in polyunsaturated fatty acids. Antioxidants are used by the food industry to delay the oxidation process. This process can be controlled by antioxidants, which may occur as natural constituents of foods or may be intentionally added to products. Synthetic antioxidants such as BHT, BHA, and propyl gallate have been extensively used as antioxidants in the industry. The worldwide tendency to avoid or minimize the use of synthetic food additives has prompted the replacement of synthetic antioxidants with natural analogues. The entire process can be supported by the detection and characterization of the reacting species by suitable application of electrospray tandem mass spectrometry under collision-induced dissociation (ESI-CID-MS/MS). Natural antioxidants were tested in this study to check the oxidative stability of algae oil when adding the natural additive. Results were observed in algae oil in situ using electrospray mass spectrometry in tandem with collision-induced dissociation tandem mass spectrometry (ESI-CID-MS/MS) and the POBN spin trapper. The results indicate that alpha-tocopherol is a better antioxidant.


Subject(s)
Antioxidants , Tandem Mass Spectrometry , Antioxidants/chemistry , Food Additives/analysis , Lipid Peroxidation , Oxidation-Reduction
2.
J Mass Spectrom ; 56(1): e4677, 2021 Jan.
Article in English | MEDLINE | ID: mdl-33448524

ABSTRACT

The kinetics of the unimolecular dissociations of proton-bound dimers produced by fast-atom bombardment from nucleosides and reference amines enables the evaluation of the proton affinities (PAs) of ribonucleosides. The PAs of cytosine, guanosine, adenosine, uridine, and deoxyuridine have been thus determined. These values and those already available for the corresponding DNA homologues allow the evaluation of the effect of the hydroxyl group in position 2' of the sugar moiety, which lowers the PAs of RNA nucleosides by 0.6-1 kcal/mol, and of the methyl group in position 5 of the thymine ring, which enhances the basicity of deoxythymidine over deoxyuridine by 0.6 kcal/mol.


Subject(s)
Nucleosides/chemistry , Spectrometry, Mass, Electrospray Ionization/methods , DNA/chemistry , Deoxyuridine/chemistry , Kinetics , Protons , RNA/chemistry , Thymidine/chemistry
3.
J Mass Spectrom ; 55(9): e4526, 2020 Sep.
Article in English | MEDLINE | ID: mdl-32567096

ABSTRACT

A fast methodology for the assay of parabens in drug and cosmetic preparations has been presented. The procedure developed is based on paper spray tandem mass spectrometry and isotope dilution approach. For each investigated paraben, the corresponding labeled standard has been used in order to improve the accuracy and reproducibility of the analyses. The MS experiments have been performed under MRM conditions, monitoring the transitions [M-H]- → m/z 92 and [M-H]- → m/z 98, respectively, for each analyte and the corresponding labeled internal standard. The quantitative assay has been performed using a calibration curve built from 2 to 15 mg/L. The method accuracy, in all case near 100%, was evaluated using fortified samples at two concentration levels, which are representative of the lower and the higher portion of calibration curve. The good values of LOQ, LOD, and reproducibility confirm the consistency of the developed approach.


Subject(s)
Cosmetics/analysis , Parabens/analysis , Pharmaceutical Preparations/analysis , Tandem Mass Spectrometry/methods , Calibration , Carbon Isotopes , Humans , Indicator Dilution Techniques , Limit of Detection , Paper , Preservatives, Pharmaceutical , Reproducibility of Results , Sensitivity and Specificity
4.
Food Chem Toxicol ; 136: 111110, 2020 Feb.
Article in English | MEDLINE | ID: mdl-31899365

ABSTRACT

A rapid analytical method for the determination of phenylethanoids content in extra virgin olive oil has been developed. The method intends to address the European regulation EU 432/2012 on health claims, which allows to report on the front label of olive oil, the positive health effects due to the consumption of this food. The innovative method is based on paper spray tandem mass spectrometry using deuterated standards. It relies on a two-step analysis, needed to assess the free form of tyrosol and hydroxytyrosol and their ester conjugates after hydrolysis treatment. Different olive oil samples have been analyzed and the classical analytical parameters such as accuracy, LOQ and LOD were calculated from fortified samples. The good values of the latters show the reliability of the new approach, that limits the time of analysis and sample preparation to few minutes.


Subject(s)
Indicator Dilution Techniques/mortality , Olive Oil/chemistry , Phenylethyl Alcohol/analogs & derivatives , Tandem Mass Spectrometry/methods , Antioxidants/chemistry , Hydrolysis , Phenylethyl Alcohol/chemistry
5.
Molecules ; 24(23)2019 Nov 28.
Article in English | MEDLINE | ID: mdl-31795131

ABSTRACT

The procedures for the extraction and separation of lipids and nutraceutics from microalgae using classic solvents have been frequently used over the years. However, these production methods usually require expensive and toxic solvents. Based on our studies involving the use of eco-sustainable methodologies and alternative solvents, we selected ethanol (EtOH) and cyclopentyl methyl ether (CPME) for extracting bio-oil and lipids from algae. Different percentages of EtOH in CPME favor the production of an oil rich in saturated fatty acids (SFA), useful to biofuel production or rich in bioactive compounds. The proposed method for obtaining an extract rich in saturated or unsaturated fatty acids from dry algal biomass is disclosed as eco-friendly and allows a good extraction yield. The method is compared both in extracted oil percentage yield and in extracted fatty acids selectivity to extraction by supercritical carbon dioxide (SC-CO2).


Subject(s)
Biological Products/isolation & purification , Biological Products/pharmacology , Lipids/isolation & purification , Lipids/pharmacology , Microalgae/chemistry , Biological Products/chemistry , Chemical Fractionation , Gas Chromatography-Mass Spectrometry , Lipids/chemistry
6.
Molecules ; 24(19)2019 Sep 25.
Article in English | MEDLINE | ID: mdl-31557931

ABSTRACT

Olive tree (Olea europaea L.) leaf, a waste by-product of the olive oil industry, is an inexpensive and abundant source of biophenols of great interest for various industrial applications in the food supplement, cosmetic, and pharmaceutical industries. In this work, the aqueous extraction of high-added value compounds from olive leaves by using microfiltered (MF), ultrapure (U), and osmosis-treated (O) water was investigated. The extraction of target compounds, including oleuropein (Olp), hydroxytyrosol (HyTyr), tyrosol (Tyr), verbascoside (Ver), lutein (Lut), and rutin (Rut), was significantly affected by the characteristics of the water used. Indeed, according to the results of liquid chromatography tandem mass spectrometry, the extracting power of microfiltered water towards rutin resulted very poor, while a moderate extraction was observed for oleuropein, verbascoside, and lutein. On the other hand, high concentrations of hydroxytyrosol were detected in the aqueous extracts produced with microfiltered water. The extraction power of ultrapure and osmosis-treated water proved to be very similar for the bio-active compounds oleuropein, verbascoside, lutein, and rutin. The results clearly provide evidence of the possibility of devising new eco-friendly strategies based on the use of green solvents which can be applied to recover bioactive compounds from olive leaves.


Subject(s)
Dietary Supplements/analysis , Olea/chemistry , Plant Extracts/chemistry , Plant Extracts/isolation & purification , Plant Leaves/chemistry , Chemical Fractionation , Chromatography, Liquid , Reproducibility of Results , Tandem Mass Spectrometry
7.
Anal Bioanal Chem ; 411(13): 2885-2890, 2019 May.
Article in English | MEDLINE | ID: mdl-30899998

ABSTRACT

Extra virgin olive oil provides an important intake of α-tocopherol, which is part of vitamin E complex. A fast analytical method for its quantification, based on paper spray mass spectrometry, has been developed. The methodology possesses the ability to record mass spectra without sample preparation or preseparation steps. The experiments were performed in Multiple Reaction Monitoring scan mode; in particular, the transitions m/z 429 → m/z 163 for α-tocopherol and m/z 435 → m/z 169 for the labeled internal standard were monitored, in order to obtain the greatest specificity and the best sensitivity. The accuracy of the method was tested analyzing spiked samples prepared at concentrations within the dynamic range of the calibration curve, which returned values near 100%. Furthermore, good values of LOQ and LOD were obtained, demonstrating that this approach can be applied for a rapid screening of tocopherols in different vegetable oils. The results were compared with analyses performed by traditional chromatographic methods. Graphical abstract.

8.
Food Chem ; 278: 261-266, 2019 Apr 25.
Article in English | MEDLINE | ID: mdl-30583372

ABSTRACT

A fast method for the determination of methylxanthines in cocoa products and drugs based on PS-MS/MS under MRM condition has been developed. Analyte ions were generated by applying a high voltage on a paper substrate drenched of sample extract using a small volume (∼15 µL) of spray solvent. The gas phase chemistry of the molecules under investigation has been elucidated. The accuracy values of the methodology ranged from 95 to 110%, while the analytical parameters LOQ, LOD, recovery and reproducibility, calculated analyzing spiked samples, confirmed the consistency of the proposed method. Furthermore, real samples have been analyzed both by the developed methodology and by using a classical HPLC-UV approach obtaining comparable values.


Subject(s)
Cacao/chemistry , Caffeine/analysis , Tandem Mass Spectrometry/methods , Theobromine/analysis , Theophylline/analysis , Chromatography, High Pressure Liquid/methods , Food Analysis/methods , Limit of Detection , Pharmaceutical Preparations/analysis , Reproducibility of Results , Tandem Mass Spectrometry/standards
10.
Biochim Biophys Acta Bioenerg ; 1859(9): 984-996, 2018 09.
Article in English | MEDLINE | ID: mdl-29626418

ABSTRACT

Here, we show that a 2:1 mixture of Brutieridin and Melitidin, termed "BMF", has a statin-like properties, which blocks the action of the rate-limiting enzyme for mevalonate biosynthesis, namely HMGR (3-hydroxy-3-methylglutaryl-CoA-reductase). Moreover, our results indicate that BMF functionally inhibits several key characteristics of CSCs. More specifically, BMF effectively i) reduced ALDH activity, ii) blocked mammosphere formation and iii) inhibited the activation of CSC-associated signalling pathways (STAT1/3, Notch and Wnt/beta-catenin) targeting Rho-GDI-signalling. In addition, BMF metabolically inhibited mitochondrial respiration (OXPHOS) and fatty acid oxidation (FAO). Importantly, BMF did not show the same toxic side-effects in normal fibroblasts that were observed with statins. Lastly, we show that high expression of the mRNA species encoding HMGR is associated with poor clinical outcome in breast cancer patients, providing a potential companion diagnostic for BMF-directed personalized therapy.


Subject(s)
Biological Products/pharmacology , Breast Neoplasms/drug therapy , Hydroxymethylglutaryl CoA Reductases/metabolism , Mevalonic Acid/metabolism , Neoplastic Stem Cells/drug effects , Plant Oils/chemistry , rho-Specific Guanine Nucleotide Dissociation Inhibitors/metabolism , Apoptosis/drug effects , Biomarkers, Tumor/metabolism , Breast Neoplasms/metabolism , Breast Neoplasms/pathology , Cell Proliferation/drug effects , Cells, Cultured , Female , Fibroblasts/cytology , Fibroblasts/drug effects , Fibroblasts/metabolism , Gene Expression Regulation, Neoplastic/drug effects , Humans , Mitochondria/drug effects , Mitochondria/metabolism , Mitochondria/pathology , Neoplasm Metastasis , Neoplastic Stem Cells/metabolism , Neoplastic Stem Cells/pathology , Prognosis , Signal Transduction/drug effects , Survival Rate
11.
Neurotoxicology ; 67: 46-53, 2018 07.
Article in English | MEDLINE | ID: mdl-29673962

ABSTRACT

Food intake ensures energy resources sufficient for basic metabolism, immune system and reproductive investment. It is already known that food-seeking performances, which are crucially controlled by orexins (ORXs), may be under the influence of environmental factors including pollutants. Among these, mancozeb (mz) is becoming an environmental risk for neurodegenerative diseases. Due to few studies on marine fish exposed to mz, it was our intention to correlate feeding latency, food intake and feeding duration to potential neurodegenerative processes in key diencephalic sites and expression changes of the ORX neuroreceptor (ORXR) in the ornate wrasses (Thalassoma pavo). Hence, fish exposed for 4 days (d) to mz 0.2 mg/l (deriving from a 0.07, 0.14, 0.2, 0.3 mg/l screening test) displayed a significant reduction (p < 0.05) of food intake compared to controls as early as 1d that became more evident (p < 0.01) after 3d. Moreover, significant enhancements of feeding latency were reported after 1d up to 3d (p < 0.001) and even feeding duration was enhanced up to 3d (p < 0.001), which instead moderately increased after 4d (p < 0.05). A reduction (-120%; p < 0.001) of mean body weight was also detected at the end of exposure. Likewise, a notable (p < 0.001) activation of ORXR protein occurred together with mRNA up-regulations in diencephalic areas such as the diffuse nucleus of the inferior lobe (+48%) that also exhibited evident degenerative neuronal fields. Overall, these results highlight an ORX role as a vital component of the neuroprotective program under environmental conditions that interfere with feeding behaviors.


Subject(s)
Feeding Behavior/drug effects , Fungicides, Industrial/toxicity , Maneb/toxicity , Neurodegenerative Diseases/chemically induced , Neurodegenerative Diseases/metabolism , Orexin Receptors/biosynthesis , Zineb/toxicity , Animals , Feeding Behavior/physiology , Female , Fishes , Gene Expression , Neurodegenerative Diseases/pathology , Orexin Receptors/genetics , Paraventricular Hypothalamic Nucleus/drug effects , Paraventricular Hypothalamic Nucleus/metabolism , Paraventricular Hypothalamic Nucleus/pathology
12.
J Chromatogr A ; 1549: 1-13, 2018 May 11.
Article in English | MEDLINE | ID: mdl-29573783

ABSTRACT

Polyamines are aliphatic amines with low molecular weight that are widely recognized as one of the most important cancer biomarkers for early diagnosis and treatment. The goal of the work herein presented is the development of a rapid and simple method for the quantification of free polyamines (i.e., putrescine, cadaverine, spermidine, spermine) and N-monoacetylated polyamines (i.e., N1-Acetylspermidine, N8-Acetylspermidine, and N1-Acetylspermine) in human urine. A preliminary derivatization with propyl chloroformate combined with the use of solid phase microextraction (SPME) allowed for an easy and automatable protocol involving minimal sample handling and no consumption of organic solvents. The affinity of the analytes toward five commercial SPME coatings was evaluated in univariate mode, and the best result in terms of analyte extraction was achieved using the divinylbenzene/carboxen/polydimethylsiloxane fiber. The variables affecting the performance of SPME analysis were optimized by the multivariate approach of experimental design and, in particular, using a central composite design (CCD). The optimal working conditions in terms of response values are the following: extraction temperature 40 °C, extraction time of 15 min and no addition of NaCl. Analyses were carried out by gas chromatography-triple quadrupole mass spectrometry (GC-QqQ-MS) in selected reaction monitoring (SRM) acquisition mode. The developed method was validated according to the guidelines issued by the Food and Drug Administration (FDA). The satisfactory performances reached in terms of linearity, sensitivity (LOQs between 0.01 and 0.1 µg/mL), matrix effect (68-121%), accuracy, and precision (inter-day values between -24% and +16% and in the range 3.3-28.4%, respectively) make the proposed protocol suitable to be adopted for quantification of these important biomarkers in urine samples.


Subject(s)
Biological Assay , Formates/chemistry , Gas Chromatography-Mass Spectrometry/methods , Polyamines/urine , Solid Phase Microextraction/methods , Adult , Female , Humans , Limit of Detection , Male , Reproducibility of Results , Sodium Chloride , Solvents , Tandem Mass Spectrometry , Temperature
13.
Anal Bioanal Chem ; 410(8): 2193-2201, 2018 Mar.
Article in English | MEDLINE | ID: mdl-29372274

ABSTRACT

A rapid and reliable method to assay the total amount of tyrosol and hydroxytyrosol derivatives in extra virgin olive oil has been developed. The methodology intends to establish the nutritional quality of this edible oil addressing recent international health claim legislations (the European Commission Regulation No. 432/2012) and changing the classification of extra virgin olive oil to the status of nutraceutical. The method is based on the use of high-performance liquid chromatography coupled with tandem mass spectrometry and labeled internal standards preceded by a fast hydrolysis reaction step performed through the aid of microwaves under acid conditions. The overall process is particularly time saving, much shorter than any methodology previously reported. The developed approach represents a mix of rapidity and accuracy whose values have been found near 100% on different fortified vegetable oils, while the RSD% values, calculated from repeatability and reproducibility experiments, are in all cases under 7%. Graphical abstract Schematic of the methodology applied to the determination of tyrosol and hydroxytyrosol ester conjugates.


Subject(s)
Antioxidants/analysis , Chromatography, High Pressure Liquid/methods , Olive Oil/analysis , Phenylethyl Alcohol/analogs & derivatives , Tandem Mass Spectrometry/methods , Chromatography, High Pressure Liquid/economics , Food Analysis/economics , Food Analysis/methods , Hydrolysis , Limit of Detection , Microwaves , Phenylethyl Alcohol/analysis , Tandem Mass Spectrometry/economics
14.
J Sep Sci ; 41(4): 929-939, 2018 Feb.
Article in English | MEDLINE | ID: mdl-29193803

ABSTRACT

In this work, a polydimethylsiloxane/divinylbenzene fiber overcoated with a layer of polydimethylsiloxane was evaluated as analytical sampling tool for the first time in human urine. Urinary polycyclic aromatic hydrocarbons with 2-6 aromatic rings were considered as target compounds. The analyte uptake in kinetic and thermodynamic regime was evaluated and compared to the performances of polydimethylsiloxane/divinylbenzene and polydimethylsiloxane fibers. The assessment of the robustness and endurance of the overcoated fiber was carried out by direct immersion solid-phase microextraction in undiluted urine performing up to 120 consecutive extractions. The overcoated fiber was then used to develop a fast and easy direct immersion solid-phase microextraction with gas chromatography and triple quadrupole mass spectrometry protocol for the quantification of the target polycyclic aromatic hydrocarbons. The attained values of accuracy and precision were 75-114% and 2-19%, respectively, while the limits of quantification ranged between 0.05 and 1 ng/L. The proposed protocol was applied to the screening of urine samples collected from smoking and nonsmoking volunteers. The successful results obtained by using the overcoated fiber create not only new alternatives for polycyclic aromatic hydrocarbon exposure assessment but also new perspectives for the application of direct immersion solid-phase microextraction to the analysis of bioclinical matrixes.


Subject(s)
Polycyclic Aromatic Hydrocarbons/urine , Solid Phase Microextraction , Adult , Gas Chromatography-Mass Spectrometry , Healthy Volunteers , Humans , Young Adult
15.
Chem Cent J ; 11(1): 111, 2017 Nov 02.
Article in English | MEDLINE | ID: mdl-29098462

ABSTRACT

This work compares the composition at different temperatures of gaseous phase of bergamot essential oil at equilibrium with the liquid phase. A new GC-MS methodology to determine quantitatively the volatile aroma compounds was developed. The adopted methodology involved the direct injection of headspace gas into injection port of GC-MS system and of known amounts of the corresponding authentic volatile compounds. The methodology was validated. This study showed that gaseous phase composition is different from that of the liquid phase at equilibrium with it.

16.
Anal Bioanal Chem ; 409(30): 7105-7120, 2017 Dec.
Article in English | MEDLINE | ID: mdl-29032454

ABSTRACT

In this work, organophosphate ester flame retardant (OPFRs) assay in environmental waters was addressed by using microextraction by packed sorbent (MEPS) and gas chromatography-tandem mass spectrometry (GC-MS/MS). Ten OPFRs with different physicochemical properties were taken into account as target compounds for a comprehensive method evaluation. Five MEPS cartridges (i.e., C2, C8, C18, Silica, and DVB) and seven solvents (i.e., methanol, ethyl acetate, methyl tert-butyl ether, hexane, acetonitrile, dichloromethane, and trichloromethane) were surveyed. The analysis was performed by using a gas chromatograph equipped with a programmed temperature vaporization injector (PTV). Univariate and multivariate approaches were exploited in order to optimize the parameters affecting the MEPS extraction and the PTV injection of the analytes into the gas chromatographic system. The optimal working conditions were achieved using DVB as sorbent material and acetonitrile as elution solvent. Internal standard calibration was carried out using TBP-d27 and TCEP-d12. Satisfactory values of accuracy and precision were generally obtained as well as limit of detection (2.7-99 pg/mL for tap water; 2.9-97 pg/mL for river water; 3-107 pg/mL for wastewater) and limit of quantification (0.01-0.2 ng/mL). The proposed protocol was evaluated on real case scenarios by analyzing tap water, river water and simulated wastewater samples. The developed method is not only eco-friendly due to the low use of organic solvents but also simple and automatable since the MEPS extraction procedure can be implemented in the autosampler routine. Graphical abstract The steps of the analytical protocol.

17.
Food Chem ; 229: 354-357, 2017 Aug 15.
Article in English | MEDLINE | ID: mdl-28372185

ABSTRACT

A rapid analytical approach for the assay of resveratrol in red wines, based on Paper Spray Mass Spectrometry (PS-MS) and Multiple Reaction Monitoring (MRM) is described. The assay involves the use of the stable isotope dilution method. The analytical parameters calculated analyzing fortified samples confirm the reliability of the proposed approach, with accuracy values about 100%, and LOD and LOQ values calculated at 0.5 and 0.8µg/mL, respectively. Furthermore, both the recovery, which was quantitative for the analyte, and the reproducibility (RSD%), checked on different days on the same wine, always below 7%, highlighted the consistency of the methodology.


Subject(s)
Isotopes/analysis , Stilbenes/therapeutic use , Tandem Mass Spectrometry/methods , Wine/analysis , Resveratrol , Stilbenes/administration & dosage
18.
Toxicol Appl Pharmacol ; 323: 26-35, 2017 05 15.
Article in English | MEDLINE | ID: mdl-28330765

ABSTRACT

The pesticide mancozeb (mz) is recognized as a potent inducer of oxidative stress due to its ability to catalyze the production of reactive oxygen species plus inhibiting mitochondrial respiration thus becoming an environmental risk for neurodegenerative diseases. Despite numerous toxicological studies on mz have been directed to mammals, attention on marine fish is still lacking. Thus, it was our intention to evaluate neurobehavioral activities of ornate wrasses (Thalassoma pavo) exposed to 0.2mg/l of mz after a preliminary screening test (0.07-0.3mg/l). Treated fish exhibited an evident (p<0.001) latency to reach T-maze arms (>1000%) while exploratory attitudes (total arm entries) diminished (-50%; p<0.05) versus controls during spontaneous exploration tests. Moreover, they showed evident enhancements (+111%) of immobility in the cylinder test. Contextually, strong (-88%; p<0.01) reductions of permanence in light zone of the Light/Dark apparatus along with diminished crossings (-65%) were also detected. Conversely, wrasses displayed evident enhancements (160%) of risk assessment consisting of fast entries in the dark side of this apparatus. From a molecular point of view, a notable activation (p<0.005) of the brain transcription factor pCREB occurred during mz-exposure. Similarly, in situ hybridization supplied increased HSP90 mRNAs in most brain areas such as the lateral part of the dorsal telencephalon (Dl; +68%) and valvula of the cerebellum (VCe; +35%) that also revealed evident argyrophilic signals. Overall, these first indications suggest a possible protective role of the early biomarkers pCREB and HSP90 against fish toxicity.


Subject(s)
Behavior, Animal/drug effects , Brain/drug effects , Cyclic AMP Response Element-Binding Protein/metabolism , Fish Proteins/metabolism , Fishes/metabolism , Fungicides, Industrial/toxicity , HSP90 Heat-Shock Proteins/metabolism , Maneb/toxicity , Nerve Degeneration , Neurotoxicity Syndromes/etiology , Water Pollutants, Chemical/toxicity , Zineb/toxicity , Animals , Brain/metabolism , Brain/pathology , Brain/physiopathology , Exploratory Behavior/drug effects , Female , Fish Proteins/genetics , Fishes/genetics , HSP90 Heat-Shock Proteins/genetics , Motor Activity/drug effects , Neurotoxicity Syndromes/metabolism , Neurotoxicity Syndromes/pathology , Neurotoxicity Syndromes/psychology , Reaction Time/drug effects , Time Factors
19.
Oncoscience ; 3(7-8): 220-241, 2016.
Article in English | MEDLINE | ID: mdl-27713912

ABSTRACT

Prostate cancer (PCa) is the sixth highest causes of cancer-related deaths in men. The molecular events underlying its behavior and evolution are not completely understood. Prostate-specific antigen (PSA) is the only approved Food and Drug Administration biomarker. A panel of ten stage-specific tumoral and adjacent non tumoral tissues from patients affected by PCa (Gleason score 6, 3+3; PSA 10 ÷19 ng/ml) was investigated by MS-based proteomics approach. The proposed method was based on identifying the base-soluble proteins from tissue, established an efficient study, which lead to a deeper molecular perspective understanding of the PCa. A total of 164 proteins were found and 132 of these were evaluated differentially expressed in tumoral tissues. The Ingenuity Pathway Analysis (IPA) showed that among all dataset obtained, 105 molecules were involved in epithelial neoplasia with a p-value of 3.62E-05, whereas, only 11 molecules detected were ascribed to sentinel tissue and bodily fluids.

20.
J Mass Spectrom ; 51(9): 761-7, 2016 Sep.
Article in English | MEDLINE | ID: mdl-27460885

ABSTRACT

A novel approach for the rapid discrimination of bergamot essential oil from other citrus fruits oils is presented. The method was developed using paper spray mass spectrometry (PS-MS) allowing for a rapid molecular profiling coupled with a statistic tool for a precise and reliable discrimination between the bergamot complex matrix and other similar matrices, commonly used for its reconstitution. Ambient mass spectrometry possesses the ability to record mass spectra of ordinary samples, in their native environment, without sample preparation or pre-separation by creating ions outside the instrument. The present study reports a PS-MS method for the determination of oxygen heterocyclic compounds such as furocoumarins, psoralens and flavonoids present in the non-volatile fraction of citrus fruits essential oils followed by chemometric analysis. The volatile fraction of Bergamot is one of the most known and fashionable natural products, which found applications in flavoring industry as ingredient in beverages and flavored foodstuff. The development of the presented method employed bergamot, sweet orange, orange, cedar, grapefruit and mandarin essential oils. PS-MS measurements were carried out in full scan mode for a total run time of 2 min. The capability of PS-MS profiling to act as marker for the classification of bergamot essential oils was evaluated by using multivariate statistical analysis. Two pattern recognition techniques, linear discriminant analysis and soft independent modeling of class analogy, were applied to MS data. The cross-validation procedure has shown excellent results in terms of the prediction ability because both models have correctly classified all samples for each category. Copyright © 2016 John Wiley & Sons, Ltd.


Subject(s)
Mass Spectrometry/methods , Oils, Volatile/analysis , Plant Oils/analysis , Oils, Volatile/chemistry , Plant Oils/chemistry , Principal Component Analysis , Reproducibility of Results , Sensitivity and Specificity
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