The consumption of illicit drugs represents a global social and economic problem. Using suitable ... more 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 UPLC–ESI-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 th...
The investigation focused on the deterioration of the walls in the hypogeum of “San Pietro Barisa... more The investigation focused on the deterioration of the walls in the hypogeum of “San Pietro Barisano” rupestrian church, located in the Matera-Sassi (Southern Italy), one of the UNESCO World Heritage sites. The study evaluated the biocide activity of a mixture of natural glycoalkaloids (GAs) extracted from the unripe fruit of Solanum nigrum and applied to clean a hypogeum wall surface in the church affected by bio-patinas. The analyzed bio-patina, collected before treatment and, at pre-established times, after treatment, showed changes in chemical composition detected by XPS, accompanied by visible discoloration and biological activity variation. The biocidal action of the glycoalkaloids mixture, directly employed on the wall surface, was effective after about four weeks for most bio-patina colonizers but not for the fungal species that can migrate and survive in the porosities of the calcarenite. Consequently, the cleaning procedure requires the integration of fungicidal actions, co...
The development and application of advanced analytical methods for a comprehensive analysis of Ca... more The development and application of advanced analytical methods for a comprehensive analysis of Cannabis sativa L. extracts plays a pivotal role in order to have a reliable evaluation of their chemotype definition to guarantee the efficacy and safety in pharmaceutical use. This paper deals with the qualitative and quantitative determination of cannabidiol (CBD), tetrahydrocannabinol (THC), cannabinol (CBN), tetrahydrocannabivarin (THCV), cannabidivarin (CBDV), and cannabigerol (CBG) based on a liquid chromategraphy-mass spectrometry (LC-MS) method using electrospray ionization in positive mode (ESI+), coupled with a hybrid quadrupole linear ion trap (LTQ) and Fourier transform ion cyclotron resonance mass spectrometer (FTICR-MS). For the first time, structural information of phytocannabinoids is available upon precursor ions’ isolation within the FTICR trapping cell and subsequent fragmentation induced by infrared multiphoton dissociation (IRMPD). Such fragmentation and accurate mass...
Stability and removal of anti-inflammatory dexamethasone sodium phosphate (DSP), anti-anxiety dru... more Stability and removal of anti-inflammatory dexamethasone sodium phosphate (DSP), anti-anxiety drug diazepam (valium) and spironolactone (SP) from wastewater produced at Al-Quds University Campus were investigated. Kinetic studies in both pure water (abiotic degradation) and in sludge (biodegradability) at room temperature were investigated. They demonstrated that DSP underwent degradation to its hydrolytic derivative, simply named dexamethasone, in both media. The first order hydrolysis rate of DSP in activated sludge at 25°C (3.80×10-6 s -1 ) was about 12-fold greater than in pure water (3.25×10-7 s -1 ). Diazepam showed high chemical stability toward degradation in pure water, and underwent faster biodegradation in sludge providing two main degradation products. The degradation reactions in sludge and pure water showed first order kinetics with rate constant values of 2.6 × 10-7 s -1 and 9.08 × 10-8 s -1 , respectively. The potassium-sparing diuretic (water pill) SP underwent degr...
ODTMA-micelle-clay complex as an efficient adsorbent was prepared from a cationic surfactant, oct... more ODTMA-micelle-clay complex as an efficient adsorbent was prepared from a cationic surfactant, octadecyltrimethylammonium (ODTMA) and a negatively charged clay (montmorillonite). It is characterized with a positive charge and large hydrophobic sites. The micelle- clay complex was investigated towards removal of the ant-inflammatory drugs (NSAIDs), Diclofenac and Naproxen and a heavy metal Cr (VI) as part of comprehensive evaluation study to utilize this adsorbent in advanced wastewater treatment technology. Stability studies demonstrated that while Diclofenac potassium was completely stable in fresh water and in sludge Naproxen underwent biodegradation in sludge to provide O-desmethyl naproxen (DMN) as its single metabolite. Al-Quds Wastewater Treatment Plant (WWTP) which includes ultrafiltration (UF) (hollow fiber HF and spiral wound SW) membranes, activated carbon (AC) and reverse osmosis (RO) has demonstrated high removal efficiency toward these two NSAIDs and Naproxen metabolite ...
Crude oil can undergo biotic and abiotic transformation processes in the environment. This articl... more Crude oil can undergo biotic and abiotic transformation processes in the environment. This article deals with the fate of an Italian crude oil under simulated solar irradiation to understand (i) the modification induced on its composition by artificial ageing and (ii) the transformations arising from different advanced oxidation processes (AOPs) applied as oil-polluted water remediation methods. The AOPs adopted were photocatalysis, sonolysis and, simultaneously, photocatalysis and sonolysis (sonophotocatalysis). Crude oil and its water-soluble fractions underwent analysis using GC-MS, liquid-state 1H-NMR, Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR-MS), and fluorescence. The crude oil after light irradiation showed (i) significant modifications induced by the artificial ageing on its composition and (ii) the formation of potentially toxic substances. The treatment produced oil oxidation with a particular effect of double bonds oxygenation. Non-polar compound...
Synthetic insecticides are widely used for crop protection both in the fields and in the food sto... more Synthetic insecticides are widely used for crop protection both in the fields and in the food stored facilities. Due to their toxicity, and assumptions of Integrated Pest Management, we conducted two independent experiments, where we studied the influence of Solanum nigrum unripe fruit extract on the toxicity of an organophosphorus insecticide fenitrothion. In the first variant of the experiment, Tenebrio molitor larvae were fed with blended fenitrothion (LC50) and the extract in four concentrations (0.01, 0.1, 1 and 10%) in ratio 1:1 for 3 days. In the second variant, a two-day application of fenitrothion (LC40) was preceded by a one-day extract treatment. The first variant did not show any increase in lethality compared to fenitrothion; however, ultrastructure observations exhibited swollen endoplasmic reticulum (ER) membranes in the midgut and nuclear and cellular membranes in the fat body, after application of blended fenitrothion and extract. An increased amount of heterochroma...
Background: Solanaceae plants produce glycoalkaloids (GAs) that affect various physiological proc... more Background: Solanaceae plants produce glycoalkaloids (GAs) that affect various physiological processes of herbivorous insects and they are being tested as potential alternatives for synthetic pesticides. They cause lethal and sublethal effects. Nevertheless, their mode of action remains unclear. Therefore, we examined the effects of Solanum nigrum fruit extracts and pure glycoalkaloids on a model beetle, Tenebrio molitor. Methods: Plant extracts or pure alkaloids were added to the food of the larvae for three days. The lipid, glycogen, and protein content in the fat body and the midgut were determined, and the contractility of the heart, hindgut, and oviduct muscles was tested using the video-microscopy technique. Finally, the ultrastructure of the fat body and the midgut was observed using electron microscopy. Results: No lethal effects were noted. Sublethal changes were observed in the content of biomolecules, malformations of organelles, chromatin condensation, and heart and ovid...
Only a small percentage of insect species are pests. However, pest species cause significant loss... more Only a small percentage of insect species are pests. However, pest species cause significant losses in agricultural and forest crops, and many are vectors of diseases. Currently, many scientists are focused on developing new tools to control insect populations, including secondary plant metabolites, e.g., alkaloids, glycoalkaloids, terpenoids, organic acids and alcohols, which show promise for use in plant protection. These compounds can affect insects at all levels of biological organization, but their action generally disturbs cellular and physiological processes, e.g., by altering redox balance, hormonal regulation, neuronal signalization or reproduction in exposed individuals. Secondary plant metabolites cause toxic effects that can be observed at both lethal and sublethal levels, but the most important effect is repellence. Plants from the Solanaceae family, which contains numerous economically and ecologically important species, produce various substances that affect insects b...
The usage of insects as model organisms is becoming more and more common in toxicological, pharma... more The usage of insects as model organisms is becoming more and more common in toxicological, pharmacological, genetic and biomedical research. Insects, such as fruit flies (Drosophila melanogaster), locusts (Locusta migratoria), stick insects (Baculum extradentatum) or beetles (Tenebrio molitor) are used to assess the effect of different active compounds, as well as to analyse the background and course of certain diseases, including heart disorders. The goal of this study was to assess the influence of secondary metabolites extracted from Solanaceae and Brassicaceae plants: Potato (Solanum tuberosum), tomato (Solanum lycopersicum), black nightshade (Solanum nigrum) and horseradish (Armoracia rusticana), on T. molitor beetle heart contractility in comparison with pure alkaloids. During the in vivo bioassays, the plants glycoalkaloid extracts and pure substances were injected at the concentration 10−5 M into T. molitor pupa and evoked changes in heart activity. Pure glycoalkaloids cause...
Diterpenoid alkaloids are natural compounds having complex structural features with many stereo-c... more 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 i...
The evolutionary arms race between plants and herbivores has led, over millions of years, to the ... more The evolutionary arms race between plants and herbivores has led, over millions of years, to the production of many substances that prevent plants from being over-eaten by plant-feeding animals [...]
The consumption of illicit drugs represents a global social and economic problem. Using suitable ... more 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 UPLC–ESI-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 th...
The investigation focused on the deterioration of the walls in the hypogeum of “San Pietro Barisa... more The investigation focused on the deterioration of the walls in the hypogeum of “San Pietro Barisano” rupestrian church, located in the Matera-Sassi (Southern Italy), one of the UNESCO World Heritage sites. The study evaluated the biocide activity of a mixture of natural glycoalkaloids (GAs) extracted from the unripe fruit of Solanum nigrum and applied to clean a hypogeum wall surface in the church affected by bio-patinas. The analyzed bio-patina, collected before treatment and, at pre-established times, after treatment, showed changes in chemical composition detected by XPS, accompanied by visible discoloration and biological activity variation. The biocidal action of the glycoalkaloids mixture, directly employed on the wall surface, was effective after about four weeks for most bio-patina colonizers but not for the fungal species that can migrate and survive in the porosities of the calcarenite. Consequently, the cleaning procedure requires the integration of fungicidal actions, co...
The development and application of advanced analytical methods for a comprehensive analysis of Ca... more The development and application of advanced analytical methods for a comprehensive analysis of Cannabis sativa L. extracts plays a pivotal role in order to have a reliable evaluation of their chemotype definition to guarantee the efficacy and safety in pharmaceutical use. This paper deals with the qualitative and quantitative determination of cannabidiol (CBD), tetrahydrocannabinol (THC), cannabinol (CBN), tetrahydrocannabivarin (THCV), cannabidivarin (CBDV), and cannabigerol (CBG) based on a liquid chromategraphy-mass spectrometry (LC-MS) method using electrospray ionization in positive mode (ESI+), coupled with a hybrid quadrupole linear ion trap (LTQ) and Fourier transform ion cyclotron resonance mass spectrometer (FTICR-MS). For the first time, structural information of phytocannabinoids is available upon precursor ions’ isolation within the FTICR trapping cell and subsequent fragmentation induced by infrared multiphoton dissociation (IRMPD). Such fragmentation and accurate mass...
Stability and removal of anti-inflammatory dexamethasone sodium phosphate (DSP), anti-anxiety dru... more Stability and removal of anti-inflammatory dexamethasone sodium phosphate (DSP), anti-anxiety drug diazepam (valium) and spironolactone (SP) from wastewater produced at Al-Quds University Campus were investigated. Kinetic studies in both pure water (abiotic degradation) and in sludge (biodegradability) at room temperature were investigated. They demonstrated that DSP underwent degradation to its hydrolytic derivative, simply named dexamethasone, in both media. The first order hydrolysis rate of DSP in activated sludge at 25°C (3.80×10-6 s -1 ) was about 12-fold greater than in pure water (3.25×10-7 s -1 ). Diazepam showed high chemical stability toward degradation in pure water, and underwent faster biodegradation in sludge providing two main degradation products. The degradation reactions in sludge and pure water showed first order kinetics with rate constant values of 2.6 × 10-7 s -1 and 9.08 × 10-8 s -1 , respectively. The potassium-sparing diuretic (water pill) SP underwent degr...
ODTMA-micelle-clay complex as an efficient adsorbent was prepared from a cationic surfactant, oct... more ODTMA-micelle-clay complex as an efficient adsorbent was prepared from a cationic surfactant, octadecyltrimethylammonium (ODTMA) and a negatively charged clay (montmorillonite). It is characterized with a positive charge and large hydrophobic sites. The micelle- clay complex was investigated towards removal of the ant-inflammatory drugs (NSAIDs), Diclofenac and Naproxen and a heavy metal Cr (VI) as part of comprehensive evaluation study to utilize this adsorbent in advanced wastewater treatment technology. Stability studies demonstrated that while Diclofenac potassium was completely stable in fresh water and in sludge Naproxen underwent biodegradation in sludge to provide O-desmethyl naproxen (DMN) as its single metabolite. Al-Quds Wastewater Treatment Plant (WWTP) which includes ultrafiltration (UF) (hollow fiber HF and spiral wound SW) membranes, activated carbon (AC) and reverse osmosis (RO) has demonstrated high removal efficiency toward these two NSAIDs and Naproxen metabolite ...
Crude oil can undergo biotic and abiotic transformation processes in the environment. This articl... more Crude oil can undergo biotic and abiotic transformation processes in the environment. This article deals with the fate of an Italian crude oil under simulated solar irradiation to understand (i) the modification induced on its composition by artificial ageing and (ii) the transformations arising from different advanced oxidation processes (AOPs) applied as oil-polluted water remediation methods. The AOPs adopted were photocatalysis, sonolysis and, simultaneously, photocatalysis and sonolysis (sonophotocatalysis). Crude oil and its water-soluble fractions underwent analysis using GC-MS, liquid-state 1H-NMR, Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR-MS), and fluorescence. The crude oil after light irradiation showed (i) significant modifications induced by the artificial ageing on its composition and (ii) the formation of potentially toxic substances. The treatment produced oil oxidation with a particular effect of double bonds oxygenation. Non-polar compound...
Synthetic insecticides are widely used for crop protection both in the fields and in the food sto... more Synthetic insecticides are widely used for crop protection both in the fields and in the food stored facilities. Due to their toxicity, and assumptions of Integrated Pest Management, we conducted two independent experiments, where we studied the influence of Solanum nigrum unripe fruit extract on the toxicity of an organophosphorus insecticide fenitrothion. In the first variant of the experiment, Tenebrio molitor larvae were fed with blended fenitrothion (LC50) and the extract in four concentrations (0.01, 0.1, 1 and 10%) in ratio 1:1 for 3 days. In the second variant, a two-day application of fenitrothion (LC40) was preceded by a one-day extract treatment. The first variant did not show any increase in lethality compared to fenitrothion; however, ultrastructure observations exhibited swollen endoplasmic reticulum (ER) membranes in the midgut and nuclear and cellular membranes in the fat body, after application of blended fenitrothion and extract. An increased amount of heterochroma...
Background: Solanaceae plants produce glycoalkaloids (GAs) that affect various physiological proc... more Background: Solanaceae plants produce glycoalkaloids (GAs) that affect various physiological processes of herbivorous insects and they are being tested as potential alternatives for synthetic pesticides. They cause lethal and sublethal effects. Nevertheless, their mode of action remains unclear. Therefore, we examined the effects of Solanum nigrum fruit extracts and pure glycoalkaloids on a model beetle, Tenebrio molitor. Methods: Plant extracts or pure alkaloids were added to the food of the larvae for three days. The lipid, glycogen, and protein content in the fat body and the midgut were determined, and the contractility of the heart, hindgut, and oviduct muscles was tested using the video-microscopy technique. Finally, the ultrastructure of the fat body and the midgut was observed using electron microscopy. Results: No lethal effects were noted. Sublethal changes were observed in the content of biomolecules, malformations of organelles, chromatin condensation, and heart and ovid...
Only a small percentage of insect species are pests. However, pest species cause significant loss... more Only a small percentage of insect species are pests. However, pest species cause significant losses in agricultural and forest crops, and many are vectors of diseases. Currently, many scientists are focused on developing new tools to control insect populations, including secondary plant metabolites, e.g., alkaloids, glycoalkaloids, terpenoids, organic acids and alcohols, which show promise for use in plant protection. These compounds can affect insects at all levels of biological organization, but their action generally disturbs cellular and physiological processes, e.g., by altering redox balance, hormonal regulation, neuronal signalization or reproduction in exposed individuals. Secondary plant metabolites cause toxic effects that can be observed at both lethal and sublethal levels, but the most important effect is repellence. Plants from the Solanaceae family, which contains numerous economically and ecologically important species, produce various substances that affect insects b...
The usage of insects as model organisms is becoming more and more common in toxicological, pharma... more The usage of insects as model organisms is becoming more and more common in toxicological, pharmacological, genetic and biomedical research. Insects, such as fruit flies (Drosophila melanogaster), locusts (Locusta migratoria), stick insects (Baculum extradentatum) or beetles (Tenebrio molitor) are used to assess the effect of different active compounds, as well as to analyse the background and course of certain diseases, including heart disorders. The goal of this study was to assess the influence of secondary metabolites extracted from Solanaceae and Brassicaceae plants: Potato (Solanum tuberosum), tomato (Solanum lycopersicum), black nightshade (Solanum nigrum) and horseradish (Armoracia rusticana), on T. molitor beetle heart contractility in comparison with pure alkaloids. During the in vivo bioassays, the plants glycoalkaloid extracts and pure substances were injected at the concentration 10−5 M into T. molitor pupa and evoked changes in heart activity. Pure glycoalkaloids cause...
Diterpenoid alkaloids are natural compounds having complex structural features with many stereo-c... more 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 i...
The evolutionary arms race between plants and herbivores has led, over millions of years, to the ... more The evolutionary arms race between plants and herbivores has led, over millions of years, to the production of many substances that prevent plants from being over-eaten by plant-feeding animals [...]
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