57 research outputs found
Mass spectrometry application on the detection of Sildenafil in aqueous phases
Sildenafil, the active ingredient of Viagra (Figure n.1), is a drug helpful in solving erectile
dysfunction problems and recently entered the list of emerging contaminants. The use of these
pharmaceuticals is increasingly widespread among perfectly healthy young people (20 or 30
years old) who make them a dangerous abuse for "recreational" purposes together with ecstasy:
the result is a synergistic amplification of their final effects, such as the feeling of euphoria,
confusion, disorientation, hallucinations, tremors or, in severe cases, irregular heartbeat and
even coma. According to the 2018 annual report prepared by the Italian Medicines Agency
(AIFA), this compoundsâ consumption had increased over time from 2.9 DDD (Defined Daily
Dose assumed per 1000 inhabitants in the referred year) in 2014 to 3.6 DDD in 2018.
Unfortunately, it is impossible to detect the actual quantity used from the population (young
and patients) because the internet network is becoming a way of purchasing to avoid medical
prescriptions. Indeed, some researchers [1] report that illicit trading with pharmaceuticals
products from the Internet is not wholly conscious of the risks for health concerning the quality
of these products, such as the possible presence of toxic impurities [2]. The increase in demand
is powering the illegal trade via the web, and, consequently, the risk of using an
ineffective/harmful to health drug is very high [3,4]. The human body does not fully utilize
these drugs. An unknown quantity, probably transformed, is excreted with urine and faeces.
The high consumption of this substance, globally accomplished by legal and illegal ways, and
the fact that Wastewater treatment plants (WWTP) cannot remove all types of contaminants
that enter the sewer legitimates thinking that they can pose a severe threat to ecosystems and
human health [5]. The unambiguous analytical determination of the active parent drug and the
identification of its transformation products are therefore indispensable to try understanding if
the quantity found of this drug in wastewater and surface water is linked to actual medical use
and to verify whether tertiary purification treatments of wastewater are effective in the removal.
In this work, the identification and quantification of this pharmaceutical product in water and
synthetic wastewater were performed by LC-ESI-LTQ/MS and confirmed by CID-MSn. Thanks
to high mass precision and MS/MS capability, determination and structural interpretation of
sildenafil and its transformation products were achieved
APPLICATION OF FTICR MASS SPECTOMETRY FOR THE EVALUATION OF LIGHT EFFECT ON POLAR COMPOUNDS IN ITALIAN CRUDE OIL
The use of the crude oil as primary source of energy has significant social and environmental impacts, from accidents and routine activities such as seismic exploration, drilling, and generation of polluting wastes. Crude oil is subject to certain degradation processes: biotic and abiotic degradation. The fate of crude oil under UV and solar irradiation was studied.
Compositions of the original and irradiated samples have been characterized by Fourier Transform Ion Cyclotron Resonance Mass Spectrometry (FT-ICR/MS) 7 T ThermoElectron that is capable of achieving the peak capacity needed to resolve individual components of a complex data matrix.
Conversion of measured masses from the IUPAC mass scale (12C = 12.00000 Da) to the Kendrick mass scale (CH2=14.00000 instead of 14.01565 Da) was performed to facilitate identification of homologous series. The van Krevelen diagram was also used for a convenient visual separation of heteroatom class and alkylation pattern.
Preliminary results shows the light influence on crude oil composition: our future work will be devoted to well understand the modification that sunlight irradiation induce on the nature of crude oil
Classification, Toxicity and Bioactivity of Natural Diterpenoid Alkaloids
Diterpenoid alkaloids are natural compounds having complex structural features with many stereo-centres originating from the amination of natural tetracyclic diterpenes and produced primarily from plants in the Aconitum, Delphinium, Consolida genera. Corals, Xenia, Okinawan/Clavularia, Alcyonacea (soft corals) and marine sponges are rich sources of diterpenoids, despite the difficulty to access them and the lack of availability. Researchers have long been concerned with the potential beneficial or harmful effects of diterpenoid alkaloids due to their structural complexity, which accounts for their use as pharmaceuticals as well as their lousy reputation as toxic substances. Compounds belonging to this unique and fascinating family of natural products exhibit a broad spectrum of biological activities. Some of these compounds are on the list of clinical drugs, while others act as incredibly potent neurotoxins. Despite numerous attempts to prepare synthetic products, this review only introduces the natural diterpenoid alkaloids, describing 'compounds' structures and classifications and their toxicity and bioactivity. The purpose of the review is to highlight some existing relationships between the presence of substituents in the structure of such molecules and their recognized bioactivity
The water we would like
Water is needed for our health: it maintains the health and integrity of every cell in the body, keeps the bloodstream liquid enough to flow through blood vessels, helps eliminate the by-products of the bodyâs metabolism, aids digestion, and other exceptional properties. High-quality water is needed to preserve health. Unfortunately, the environment and all its sectors are differently contaminated. This dangerous state is closely linked to increased anthropic activities (industrial and agricultural) and the use of harmful substances released without control. Old contaminants (pesticides and substances deriving from industrial activities) and new contaminants, called "emerging" (drugs, phytotoxins, body care products), can arrive in rivers, in surface and deep water, and the sea if they are not removed from the wastewater. These substances are harmful to human health because they enter the environment in quantities exceeding the natural self capacity purification of the ecosystems. We can be exposed to water-derived contaminants in different ways. For example, people can ingest small amounts of pollutants by drinking water; they can absorb pollutants through the skin while bathing or showering and during recreational activities, such as swimming, windsurfing, and water skiing; they can inhale droplets suspended in the air or vapors while taking a shower. They can also ingest foods that have been contaminated with water-borne pollutants.Wastewater treatment plants (WWTPs) cannot altogether remove most of these substances, which can easily reach the drinking water supplies, causing health problems for adults and children. Although drinking water quality is regulated and monitored in many countries, todayâs increased knowledge suggests reviewing standards and guidelines on a near-permanent basis for both held and newly identified contaminants and adopting technologies as tertiary treatment processes, which could promote the easy degradation of recalcitrant compounds. It will be necessary to verify that the degradation products are less dangerous than the original molecules and that no dangerous aggregation products are formed. This communication reports some of the degradation studies carried out by our Research Teams in collaboration with foreign researchers using Advanced Oxidation Processes (AOPs) on pesticides and pharmaceuticals present in actual water samples. Photolysis and heterogeneous photocatalysis under simulated solar irradiation using two forms of TiO2 (suspended or immobilized on the surface of thin glass plates) have been investigated to assess the suitability of different oxidation processes to promote mineralization of recalcitrant substances. Transformation products (TPs) have been identified by an LC system coupled to a hybrid LTQ-FTICR (7-T) mass spectrometer (MS). To evaluate the treatment methods' effectiveness, the treated solutions' measurements have been performed using the âMicrotoxÂź Toxicity Testâ that reports the luminescence inhibition of the marine bacteria Vibrio fischeri. During the degradation process, the temporary formation of toxic fragments was observed, which rapidly degraded to complete mineralization. Samples collected during the degradation process showed the temporary toxicity of the water. The rate of decomposition was highly dependent on the method used. Advanced oxidation processes such as TiO2/Xe-arc system, lead to a rapid decrease of the biorecalcitrant chemical concentrations in aqueous solutions, while photolysis and TiO2-coated glass are less effective. These promising results push us to continue and improver experimental trials. What is the future prospect? The creation of prototypes to be used by farmers and artisans to start with the virtuous path of water recycle
Detection of Eight Cannabinoids and One Tracer in Wastewater and River Water by SPE-UPLCâESI-MS/MS
The consumption of illicit drugs represents a global social and economic problem. Using suitable analytical methods, monitoring, and detection of different illegal drugs residues and their metabolites in wastewater samples can help combat this problem. Our article defines a method to develop, validate, and practically applicate a rapid and robust analytical process for the evaluation of six naturally occurring cannabinoids (CBG, CBD, CBDV, CBN, THC, THCV), two cannabinoids in acidic form (CBDA, THCA-A), and the major cannabis-related human metabolite (THC-COOH). After SPE offline enrichment, we used a UPLCâESI-MS/MS system, which permitted the determination of several by-products. Studied matrices were samples of different origins: (i) effluent water from a wastewater treatment plant in the Porto urban area; (ii) environmental water from Febros River, the last left-bank tributary of the Douro River. The multi-residue approach was substantiated and successfully employed to analyze the water samples collected in the above locations. The rapid and precise quantification of nine different cannabinoids in different water samples occurred within nine minutes at the ng Lâ1 level. The appearance of dozens of ng Lâ1 of some cannabis secondary metabolites, such as CBD, CBDA, CBN, THCA-A, indicates this plant speciesâ widespread usage among the general population in the considered area
The impact of COVID-19 on radiological findings in patients accessing the emergency department: a multicentric study
The aim of this multicentric study is to illustrate how the COVID-19 pandemic lockdown affected the workload and outcomes of radiological examinations in emergency radiology
Identification and antimicrobial activity of most representative secondary metabolites from different plant species
Abstract Background The plant kingdom constitutes an enormous reservoir of bioactive molecules, generally used by plants to prevent or to protect themselves from pathogens' attacks. To date, several primary or secondary plant metabolites have been already proven to exert antibiotic activities; nonetheless, researchers are still continuing to lavish great efforts to identify and characterize new natural molecules one by one. Aiming at the replacement of synthetic chemical products, the bioactivity of plant extracts should be assessed case by case, and active substances should be tested as individuals to obtain accurate information on the real usefulness of plant metabolites. In this work major glycoalkaloids obtained from Solanum nigrum, glucosinolates from Armoracia rusticana, and cannabinoids from Cannabis sativa were identified. The antimicrobial activity of crude extracts and pure components against Gram+ (Bacillus cereus (A1I), Bacillus thuringiensis (B7I2), and Bacillus amyloliquefaciens (A5TI)) and Gramâ bacteria (Pseudomonas orientalis (A14-1II), and Stenotrophomonas maltophilia (B9TIII)), employed as model organisms, was tested. Result Major glycoalkaloids, glucosinolates, and cannabinoids were identified in crude plants' extracts using high-resolution LCâESI-FTICR/MS. From antimicrobial assays useful information towards a few of biological activities of crude extracts and individual components were obtained. Solanum nigrum extracts revealed inhibition activity on all bacteria tested as well as the main active glycoalkaloids, solamargine and solasonine, which were found to be active even when tested individually. At assayed concentrations, A. rusticana extract was active towards a few of the microorganisms tested, confirming that the activity of glucosinolates can be referred only partially to the mother molecules, while biological efficiency of such kind of compounds is mainly due to their enzymatic breaking off, where myrosinase converts them into isothiocyanates and/or thiocyanates. Hemp-type C. sativa extract showed antimicrobial activity only against Gram+ bacteria, but the main individual components tested showed always a limited bioactivity. Conclusion Promising results were obtained, but tests performed in vitro are only the first step of a wider investigation as required for an extensive application. Further research efforts are necessary to demonstrate the efficiency of natural substances in different target environments
An Interplay between a Face-Centred Composite Experimental Design and Solid-Phase Microextraction for Wine Aroma GC/MS Analysis
For oenological products, most of the intrinsic and extrinsic drivers of perceived quality are associated with specific aromatic profiles. Aromatic diversity has been recognized as a central element in perceived quality as it is able to transmit the complex interactions between grape variety, geographical characteristics, and viticultural and winemaking practices, including the fermentative process. A comprehensive characterization of flavour compounds by headspace solid-phase microextraction (HS-SPME) and gas chromatography coupled to mass spectrometric analysis is often needed in order to ascertain the quality of wine. HS-SPME requires a proper optimization that can be achieved through an adequate experimental design. Here, a HS-SPME/GC-MS based method was developed to investigate the volatile compounds of wine samples obtained by laboratory-scale fermentations. This was performed by inoculating a commercial Saccharomyces cerevisiae strain, which is used both as single starter and as mixed starter, with an indigenous Hanseniaspora osmophila strain. The experimental conditions of HS-SPME (extraction temperature and time) were optimized by applying a face-centred composite experimental design. Up to 95% of the total variance was explained by the proposed model. The optimized method allowed us to confirm the usefulness of combining the inoculation of grapes with selected yeast strains in co-culture situations in order to improve the wine bouquet
Development and Validation of a Reversed-Phase HPLC Method with UV Detection for the Determination of L-Dopa in Vicia faba L. Broad Beans
L-Dopa (LD), a substance used medically in the treatment of Parkinson's disease, is found in several natural products, such as Vicia faba L., also known as broad beans. Due to its low chemical stability, LD analysis in plant matrices requires an appropriate optimization of the chosen analytical method to obtain reliable results. This work proposes an HPLC-UV method, validated according to EURACHEM guidelines as regards linearity, limits of detection and quantification, precision, accuracy, and matrix effect. The LD extraction was studied by evaluating its aqueous stability over 3 months. The best chromatographic conditions were found by systematically testing several C-18 stationary phases and acidic mobile phases. In addition, the assessment of the best storage treatment of Vicia faba L. broad beans able to preserve a high LD content was performed. The best LD determination conditions include sun-drying storage, extraction in HCl 0.1 M, chromatographic separation with a Discovery C-18 column, 250 x 4.6 mm, 5 mu m particle size, and 99% formic acid 0.2% v/v and 1% methanol as the mobile phase. The optimized method proposed here overcomes the problems linked to LD stability and separation, thus contributing to the improvement of its analytical determination
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Glucosinolates, myrosinase hydrolysis products, and flavonols found in rocket (Eruca sativa and Diplotaxis tenuifolia)
Rocket species have been shown to have very high concentrations of glucosinolates and flavonols, which have numerous positive health benefits with regular consumption. In this review we highlight how breeders and processors of rocket species can utilize genomic and phytochemical research to improve varieties and enhance the nutritive benefits to consumers. Plant breeders are increasingly looking to new technologies such as HPLC, UPLC, LC-MS and GC-MS to screen populations for their phytochemical content to inform plant selections. Here we collate the research that has been conducted to-date in rocket, and summarise all glucosinolate and flavonol compounds identified in the species. We emphasize the importance of the broad screening of populations for phytochemicals and myrosinase degradation products, as well as unique traits that may be found in underutilized gene bank resources. We also stress that collaboration with industrial partners is becoming essential for long-term plant breeding goals through research
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