Macrocapsules, composed of a pH-sensitive polymer and phosphate buffer, offer a novel remediation alternative for acidic ground waters. To test their potential effectiveness, laboratory experiments were carried out followed by a field trial within a coal pile runoff (CPR) acidic contaminant plume. Results of traditional limestone and macrocapsule treatments were compared in both laboratory and field experiments. Macrocapsules were more effective than limestone as a passive treatment for raising pH in well water from 2.5 to 6 in both laboratory and field experiments. The limestone treatments had limited impact on pH, only increasing pH as high as 3.3, and armoring by iron was evident in the field trial. Aluminum, iron and sulfate concentrations remained relatively constant throughout the experiments, but phosphate increased (0.15-32 mg/L), indicating macrocapsule release. This research confirmed that macrocapsules may be an effective alternative to limestone to treat highly acidic ground water. Encapsulated phosphate buffer macrocapsules were more effective than limestone for passive treatment of acidic coal pile runoff (CPR) contaminated ground water, increasing pH from 2.5 to 6 in laboratory and field experiments.

The aims of the present study were to optimize and validate methods for esterase activity (EA), total oxidant status (TOS) and total antioxidant capacity (TAC) determination in mussel' gills, and to establish the relationships between these biomarkers and Pb, Cd and Cu pollution, in single form and ternary mixture. Two different buffers for sample homogenization, the need of ultracentrifugation, and analytical validation were evaluated. Coefficients of variation, when buffer without additives and ultracentrifugation were used, were <15%, and recovery were 97%–109% in all cases. The EA response tends to decrease with treatments, TOS decreased significantly in Cd and ternary groups, while TAC tended to increase in treatments with Pb, Cd and ternary groups. In conclusion, the methods for EA, TOS and TAC measurements in gills of mussel were precise and accurate and could be interesting resources in biomonitoring programmes.

Albendazole (ALB) belongs to a group of benzimidazoles - classified as antiparasitic pharmaceuticals. Its widespread application results in the presence of this pharmaceutical in natural environment (water and soil). In this paper a suitable pretreatment method was established including sampling, freeze-drying and extraction. Vicia faba was used as model organism. ALB accumulation by plant tissues was observed in hydroponic culture as well as in soil. The range of pharmaceutical concentrations was 1.7 × 10-5 mol/L (in hydroponic culture) and 1.7 × 10-5 to 1.7 × 10-4 mol/kg air dry soil (in soil). Observations were conducted for 14 days. After this time biological material was freeze-dried and after homogenization, dimethyl sulfoxide (DMSO) extraction was performed. The recovery of ALB for the roots was 93 % while for the shoots 86 %. After cleaning, the samples were subjected to further analysis by HPLC system. Phosphate buffer and acetonitrile (50:50) were used as a mobile phase. Drug retention time was 6.3 min. Results obtained in this experiment indicate higher drug accumulation in roots rather than in the hypocotyl part of the plant, cultivated both in soil and in hydroponic culture. © 2013 The Author(s).

Extraction and analysis methods have been developed for the detection of the following four antibacterial agents and two natural estrogens in treated municipal wastewater sludge and commercial compost: sulfamethoxazole (SMX), sulfadimethoxine (SDM), tetracycline (TET), oxytetracycline (OXY), estrone (E1), and 17β-estradiol (E2). The antibiotics and estrogens were extracted from secondary sludge and mixed compost using ultrasonic solvent extraction. Citric acid (pH 4.7) and methanol were used as extraction buffer, followed by tandem-solid-phase extraction cleanup, strong anion exchange + hydrophilic–lipophilic balance for antibiotics and CarboPrep/NAX for estrogens. For quantification, two different methods were employed, using HPLC–MS/MS, with an electrospray ionization source for antibiotics and an atmospheric-pressure chemical ionization source for estrogens. Recoveries were 11–31% for the sulfonamides (SMX and SDM) and tetracyclines (TET and OXY) and 30–59% for the estrogens (E1 and E2) over the entire method. Limits of detection for the extraction method were in the nanogram per gram range for dry weight sludge and compost samples. Neither of the two sulfonamide antibiotics was detected in secondary sludge or mixed compost samples. Estrogens were found in compost in amounts of 160 ± 65 ng/g (E1) and 21 ± 3 ng/g (E2), but not in sludge. The tetracyclines, as well as what is believed to be the 4-epimer of OXY, were found in both sludge and compost in amounts of 1.57 ± 0.67 and 2.95 ± 0.42 μg/g (TET), 0.56 ± 0.12 and 6.51 ± 0.52 μg/g (OXY), and 7.60 ± 1.68 and 1.35 ± 0.24 μg/g (4-epi-OXY), respectively. These results indicate that sorption-prone compounds are not removed during the wastewater treatment process and can persist through sludge digestion and that the composting process does not sufficiently eliminate these particular contaminants. Thus, biosolids (even composted) are an additional source of drug residues leaching into the environment, and it must be considered while using biosolids as fertilizer.

The use of multiwall carbon nanotubes (MWCNT) as an efficient solid extractor in preconcentration/cleanup studies for tin determination in water samples by electrothermal atomic absorption spectrometry (ETAAS) is proposed. In the proposed method, tin adsorption onto MWCNT was carried out by percolating the solution previously buffered (pH 4.79 with 0.24 mol L−1 acetic acid/acetate buffer) at 4.0-mL min−1 flow rate, followed by elution with 1.0 mL of 2.7 mol L−1 HNO3. Factors such as sample pH, preconcentration/cleanup flow rate, type and concentration of eluent, and buffer concentration were appraised and optimized from chemometric tools based on fractional factorial design and Doehlert design. A limit of detection of 0.73 μg L−1 and precision (n = 8) assessed as relative standard deviation of 8.6% and 7.0% for tin concentration of 8.0 and 43.0 μg L−1, respectively, were achieved. Foreign metallic ions (Ni2+, Pb2+, Co2+, Zn2+, Cd2+, Mn2+, and Fe3+) were checked as potential interferents, and no interference was observed up to an analyte/interference ratio of 1:10 (m/v). Direct tin determination by ETAAS in water samples containing high salt amount is drastically affected by background signal. However, previous cleanup of sample by MWCNT has promoted a significant improvement and makes the method useful for tin monitoring in water samples (mineral, lake, mine, and natural waters) by ETAAS. Quantitative recovery values ranging from 91.5% to 103.0% attested the applicability of the proposed preconcentration/cleanup for tin determination in water samples.

The present study describes the impregnation of coffee extract (CE) into bacterial cellulose synthesized from kombucha tea fungus (KBC) of different cellulose content, incubated for different incubation periods (2, 4, and 10 days), to prepare biocomposites having the potential for wound healing applications. Total polyphenols in hydroalcoholic extracts from ground roasted coffee and its release from the prepared biocomposites were determined as gallic acid equivalent. The polyphenols content was found to be 13.66 mg/g and the minimum inhibitory concentration (MIC) of the CE was determined using colony-forming unit (CFU) method against Gram-negative bacteria Escherichia coli and Gram-positive bacteria Staphylococcus aureus where the growth inhibition was 86 and 97% respectively. Biocomposites (KBC/CE) with the lowest cellulose and CE content showed the highest wet tensile stress (3.35 MPa), absorption of pseudo extracellular fluid (154.32% ± 4.84), and water vapor transmission rate (3184.94 ± 198.07 g/m²/day), whereas it showed the lowest polyphenols’ release (51.85% ± 2.94)when immersed in PBS buffer of pH 7.4. The impregnation of CE into KBC provided biocomposites that can enlarge the range of BC in the biomedical application.

In the present study, a novel synthesized adsorbent material based on 3-mercaptopropyltrimethoxysilane-functionalized multi-walled carbon nanotubes was used to increase the Pb²⁺ adsorption from aqueous solutions in a flow injection solid-phase extraction system coupled to flame atomic absorption spectrometry. Spectroscopic and microscopic techniques (Fourier transform infrared spectroscopy, energy dispersive spectroscopy, and scanning electron microscopy) were employed to confirm the chemical modification of the adsorbent surface. Preconcentration conditions (sample pH, flow rate, buffer solution, and eluent concentrations) were optimized using factorial and Doehlert matrix designs that made it possible to construct a linear graph in the 5.0- to 130.0-μg L⁻¹ range (r = 0.9999) and estimate detection and quantification limits (1.7 and 5.7 μg L⁻¹, respectively). The method precision was found to be 4.20 and 1.97 % for 5.0 and 100.0 μg L⁻¹ Pb²⁺ solutions, respectively. When using the 3-mercaptopropyltrimethoxysilane-functionalized multi-walled carbon nanotubes, the sensitivity for the Pb²⁺ trace determination was improved to 95 % compared with the oxidized multi-walled carbon nanotubes, thus evidencing the significant enhancement of the adsorption capacity. The developed method was successfully applied to the analysis of Pb²⁺ species in different water samples and the PACS-2 marine sediment-certified reference material.

The separation on microchip provides the advantages including high efficiency, increased throughput, reduced quantities of hazardous materials, cost saving, relatively facile instrumentation, improved portability, etc. A technique of micellar electrokinetic chromatography (MEKC) coupled with amperometric detection has been actualized on a polydimethylsiloxane microchip for the rapid separation and determination of three phenolic xenoestrogens as octylphenol (OP), 4-nonylphenol (4-NP), and bisphenol A (BPA). The baseline separation of these phenolic xenoestrogens is successfully obtained within 55 s under the optimized MEKC conditions with borate running buffer of pH 8.0 containing sodium dodecyl sulfate and β-cyclodextrin. The linear range for OP, 4-NP, and BPA are 20–1,000, 15–1,000, and 20–1,000 μg/L with the detection limit of 5.0, 4.0, and 3.0 μg/L, respectively. The present method is successfully applied for the determination of these phenolic xenoestrogens in some industrial wastewater samples from mainland of China with the recoveries ranged from 90.2 to 109.4 %.