Analytische Chemie
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Carbamazepine is an antiepileptic drug that can be used as a marker for the cleaning efficiency of wastewater treatment plants. Here, we present the optimization of a fast and easy on-site measurement system based on fluorescence polarization immunoassay and the successful application to wastewater. A new monoclonal highly specific anti-carbamazepine antibody was applied. The automated assay procedure takes 16 min and does not require sample preparation besides filtration. The recovery rates for carbamazepine in wastewater samples were between 60.8 and 104% with good intra- and inter-assay coefficients of variations (less than 15 and 10%, respectively). This automated assay enables for the onsite measurement of carbamazepine in wastewater treatment plants.
In the aquatic environment, pharmaceutical drugs are submitted to degradation processes, where pho-todegradation is one of the most important mechanisms affecting the fate, persistence and toxicity of thecompounds. Carbamazepine, a widely used antiepileptic, is known to suffer photodegradation in waterbodies and generate photoproducts, some of them with higher potential toxicity than the parent com-pound. Therefore, to evaluate the toxic effects of CBZ when combined with its photoproducts, an acuteexposure (96 h) with the edible clam Scrobicularia plana was performed using environmental concentra-tions of CBZ (0.00–9.00 µg/L) irradiated (and non-irradiated) with simulated solar radiation. The analysisof the irradiated CBZ solutions by mass spectrometry revealed the formation of 5 photoproducts, includ-ing acridine (a compound known to be carcinogenic). Oxidative stress results showed that the exposureto CBZ photoproducts did not increase the toxicity to clams, by comparison with the parent compound.
The catalytic efficiency of two magnetically responsive nanocatalysts was evaluated for the Degradation of Reactive Black 5 (RB5) and Reactive Yellow 84 (RY84) azo dyes using hydrogen peroxide as oxidant undervery mild conditions (atmospheric pressure, room temperature). In order to obtain the nanocatalysts, thesurface of magnetite (Fe3O4) nanoparticles, prepared by a co-precipitation method, was further modified with ferrous oxalate, a highly sensitive non-hazardous reducing agent. The sensitized nanomaterials were characterized by X-ray diffraction, scanning and transmission electron microscopy, energy-dispersive X-ray spectroscopy and vibrating sample magnetometry, and used in the catalytic wet hydrogen peroxideoxidation (CWHPO) of RB5 and RY84, in laboratory-scale experiments. The effect of important variables such as catalyst dosage, H2O2 concentration, and contact time was studied in the dye Degradation kinetics. The results showed that it was possible to remove up to 99.7% dye in the presence of 20 mM H2O2 after 240 min of oxidation for a catalyst concentration of 10 g L−1at 25◦C and initial pH value of 9.0.CWHPO of reactive dyes using sensitized magnetic nanocatalysts can be a suitable pre-treatment methodfor complete decolorization of effluents from textile dyeing and finishing processes, once the Optimum operating conditions are established.
The use of magnetic materials as heterogeneous catalysts has attracted increasing attention in the last years since they proved to be promising candidates for water treatment. In the present study, two types of surface-modified magnetite (Fe3O4) nanoparticles, coated with non-hazardous naturally occurring agents—either tannic acid (TA) or dissolved natural organic matter—were evaluated as magnetic heterogeneous catalysts. Chemical synthesis (co-precipitation) was chosen to yield the nanocatalysts due to its well-established simplicity and efficiency. Subsequently, the properties of the final products were fully assessed by various characterization techniques. The catalytic activity in heterogeneous oxidation of aqueous solutions containing a model pollutant, Bisphenol A (BPA), was comparatively studied. The effect of operational parameters (catalyst loading, H2O2 dosage, and UV light irradiation) on the Degradation performance of the oxidation process was investigated. The optimum experimental parameters were found to be 1.0 g/L of catalysts and 10 mM H2O2, under UV irradiation. The highest mineralization rates were observed for Fe3O4-TA catalyst. More than 80 % of BPA was removed after 30 min of reaction time under the specified experimental conditions. The obtained results showed that the two catalysts studied here are suitable candidates for the removal of pollutants in wastewaters by means of heterogeneous reaction using a green sustainable treatment method.
Several environmental stressors have been identified as key and/or emerging drivers of habitat change that could significantly influence marine near-shore ecosystems. These include increasing discharges of pharmaceutical contaminants into the aquatic coastal systems. Pharmaceutical drugs are often detected in aquatic environments but still information on their toxicity impacts on inhabiting species is scarce, especially when acting in combination. Furthermore, almost no information is available on the impacts of pharmaceuticals in polychaetes, often the most abundant taxon in benthic communities and commonly used as indicator species of environmental conditions. Therefore, the present study aimed to evaluate the biochemical alterations induced in the polychaete Hediste diversicolor, from a low contaminated area at the Ria de Aveiro lagoon (Portugal), by the antiepileptic drug carbamazepine (0.0 - control, 0.3, 3.0, 6.0 and 9.0 μg/L) and the stimulant caffeine (0.0 - control, 0.5, 3.0, and 18.0 μg/L), acting alone and in combination (0.3 CBZ + 0.5 CAF and 6.0 CBZ + 3.0 CAF). Glutathione Stransferases (GSTs), superoxide dismutase (SOD) and catalase (CAT) activities was determined in Hediste diversicolor from each condition. Lipid peroxidation (LPO), glutathione reduced and oxidized (GSH and GSSG), glycogen and electron transport system (ETS) were also measured. The results obtained clearly revealed that both drugs induced oxidative stress in H. diversicolor, shown by the increase on LPO levels and decrease on total glutathione and GSH/GSSG ratio with the increase of exposure concentrations. Furthermore, the present findings demonstrated that polychaetes biotransformation capacity as well as antioxidant defense mechanisms were not sufficiently efficient to fight against the excess of reactive oxygen species (ROS) leading to LPO when organisms were exposed to both drugs. Our results also demonstrated that polychaetes tended to decrease the activity of ETSwhen exposed to drugs, avoiding energy expenditurewhich may prevent them fromgreater damages. The present study further revealed that the impacts induced by the combination of both drugswere similar to those obtained at the highest drugs concentrations acting alone.
Caffeine is known to be one of the most consumed psychoactive drugs. For this reason, caffeine is continuously released into the environment with potential impacts on inhabiting organisms. The current study evaluated the biochemical alterations induced in the clam species Ruditapes philippinarum after exposure for 28 days to caffeine (0.5, 3.0 and 18.0 mg/L). The results obtained showed that, with the increasing caffeine concentrations, an increase in clams defense mechanisms (such as antioxidant and biotransformation enzymes activity) was induced which was accompanied by an increase in protein content. Nevertheless, although an increase on defense mechanisms was observed, clams were not able to prevent cells from lipid peroxidation that increased with the increase of caffeine concentration. Furthermore, with the increase of exposure concentrations, clams increased their metabolic activity (measured by electron transport activity), reducing their energy reserves (glycogen content), to fight against oxidative stress. Overall, the present study demonstrated that caffeine may impact bivalves, even at environmentally relevant concentrations, inducing oxidative stress in organisms. The present study is an important contribution to address knowledge gaps regarding the impacts of long-term exposures to pharmaceuticals since most of the studies assessed the effects after acute exposures, most of them up to 96 h.
In the last decade studies have reported the presence of several pharmaceutical drugs in aquatic environments worldwide and an increasing effort has been done to understand the impacts induced on wildlife. Among the most abundant drugs in the environment is caffeine, which has been reported as an effective chemical anthropogenic marker. However, as for the majority of pharmaceuticals, scarce information is available on the adverse effects of caffeine on marine benthic organisms, namely polychaetes which are the most abundant group of organisms in several aquatic ecossystems. Thus, the present study aimed to evaluate the biochemical alterations induced by environmentally relevant concentrations of caffeine on the polychaete species Diopatra neapolitana and Arenicola marina. The results obtained demonstrated that after 28 days exposure oxidative stress was induced in both species, especially noticed in A. marina, resulting from the incapacity of antioxidant and biotransformation enzymes to prevent cells from lipid peroxidation. The present study further revealed that D. neapolitana used glycogen and proteins as energy to develop defense mechanisms while in A. marina these reserves were maintained independently on the exposure concentration, reinforcing the low capacity of this species to fight against oxidative stress.
Ocean acidification and increasing discharges of pharmaceutical contaminants into aquatic systems are among key and/or emerging drivers of environmental change affecting marine ecosystems. A growing body of evidence demonstrates that ocean acidification can have direct and indirect impacts on marine organisms although combined effects with other stressors, namely with pharmaceuticals, have received very little attention to date. The present study aimed to evaluate the impacts of the pharmaceutical drug Carbamazepine and pH 7.1, acting alone and in combination, on the clamScrobicularia plana. For this, a long-termexposure (28 days)was conducted and a set of oxidative stress markers was investigated. The results obtained showed that S. plana was able to develop mechanisms to prevent oxidative damage when under low pH for a long period, presenting higher survival when exposed to this stressor compared to CBZ or the combination of CBZ with pH 7.1. Furthermore, the toxicity of CBZ on S. plana was synergistically increased under ocean acidification conditions (CBZ + pH 7.1): specimens survival was reduced and oxidative stress was enhanced when compared to single exposures. These findings add to the growing body of evidence that ocean acidification will act to increase the toxicity of CBZ to marine organisms,which has clear implications for coastal benthic ecosystems suffering chronic pollution from pharmaceutical drugs.
Photodegradation of organic pollutants in water by immobilized porphyrins and phthalocyanines
(2016)
New methods for water treatment are required as a result from an increasing awareness in the reduction of the pollution impact in the environment. In the perspective of the photo-oxidation of organic pollutants present in water, the principal incentive for the preparation of heterogeneous photocatalysts is their easy recovery from the reaction mixture, which allows their reuse in successive runs, minimizing the loss of their original photocatalytic properties. Different types of supports can be used in the immobilization of photoactive species, such as porphyrins (Pors) and phthalocyanines (Pcs). This mini-review will consider the different methodologies for the immobilization of Pors and Pcs and their photocatalytic performance in the photodegradation of organic pollutants in water, addressing also their recycling ability in successive water treatments.
The toxicity induced in non-target organisms by pharmaceutical drugs has been the focus of several studies. In the aquatic environment, most of the studies have been devoted to fish and bivalves, while little is known on the impacts induced in polychaetes. The present study evaluated the impacts of carbamazepine and caffeine on the regenerative capacity of Diopatra neapolitana, a polychaete species with high ecological and economic relevance. Under laboratory controlled conditions polychaetes were exposed, during 28 days, to carbamazepine (Ctl-0.0; 0.3; 3.0; 6.0; 9.0 mg/L) and caffeine (Ctl-0.0; 0.5; 3.0; 18.0 mg/L). During the experiment, at days 11, 18, 25, 32, 39 and 46 after amputation, for each specimen, the percentage of the body width regenerated was determined and the number of new segments was counted. The regenerative capacity was assessed considering the number of days needed to achieve full regeneration and the total number of new segments. The obtained results revealed that with the increase of drugs concentrations organisms regenerated less new segments and took longer to completely regenerate.
Zeolitic Imidazolate Frameworks (ZIFs) are crystalline materials
that comprise of metal nodes and Imidazole derivatives as
linkers. ZIF-67 is often used in polymer composite materials
e. g. for gas separation membranes. Post-synthesis treatment of
ZIF-67 crystals with ultrasound leads to unforeseen plasticity
that resulted in sintered ZIF-67 and ZIF-67 nano-flakes.
Consequently, ultrasound increases the external surface area of
ZIF-67 which might improve e.g. blending with polymers in
composite materials. These new morphologies of ZIF-67 were
characterized by transmission electron, scanning electron, and
atomic force microscopy. The ultrasound treatment of ZIF-67
did not result in the formation of an amorphous framework or
a meta-stable crystal structure as indicated by powder x-ray
diffraction. In addition, ultra-sonicated ZIF-67 retained the high
gas adsorption capacity and pore size compared to synthesized
ZIF-67. The morphological changes are hard to detect with
standard analytical methods that are usually utilized for MOF
characterization. These findings also suggest that sonochemical
treatment of ZIFs leads to structural effects beyond increasing
the amount of nucleation clusters during sono-chemical synthesis,
which is currently not addressed in the field.
Three types of hybrid modified magnetite (Fe₃O₄) nanoparticles, functionalized with either chitosan, chitosan/iron (II) oxalate or chitosan/iron (III) citrate, were synthesized by chemical precipitation method.
The obtained nanomaterials were characterized by energy dispersive X-ray spectroscopy, X-ray diffraction, Brunauer–Emmett–Teller analysis, scanning and Transmission electron microscopy, Fourier transform infrared spectroscopy and vibrating sample magnetometry. The prepared composites were further tested as magnetic catalysts for the removal of bisphenol A (BPA) in aqueous media. The kinetic Degradation experiments were performed at laboratory scale, while the best operational parameters for all three materials were established: 1.00 g L⁻¹ of catalyst, 10 mmol L⁻¹ H₂O₂, under simulated solar light irradiation.
After 15 min of UVA irradiation under the experimental conditions mentioned above, it was possible to decompose up to 99% of the micropollutant over all catalysts. Fe₃O₄/chitosan/iron oxalate catalyst showed the highest and fastest catalytic activity in BPA removal. Catalytic wet peroxide oxidation of non-biodegradable micropollutants on such iron-based hybrid nanoparticles can be a suitable pre-treatment method for wastewater decontamination, as an environment-friendly simplified Approach for water clean-up.
Sulfamethoxazol (SMX),a sulfonamide, is a widely used bacteriostatic antibiotic and therefore a promising marker for the entry of anthropogenic Pollution in the environment. SMX is frequently found in wastewater and surface water. This study presents the production of high affinity and selective polyclonal antibodies for SMX and the development and Evaluation of a direct competitive enzyme-linked immunosorbent assay(ELISA)for the quantification of SMX in environmental watersamples. The crystal structures of the cross-reacting compounds sulfamethizole, N4-acetyl-SMX andsuccinimidyl-SMX were determined by x-ray diffraction aiming to explain their high cross-reactivity. These crystal structures are described for the first time. The quantification range of the ELISA is 0.82–63 µg/L. To verify our results, the SMX concentration in 20 environmental samples,including wastewater and surfacewater,was determined by ELISA and tandem mass spectrometry(MS/MS).A good Agreement of the measured SMX concentrations was found with average recoveries of 97–113%for the results of ELISA compared to LC-MS/MS.