The dissemination of antibiotic resistance (AR) has attracted global attention because of the increasing antibiotic treatment failure it has caused. Through natural transformation, a live bacterium takes up extracellular DNA (exDNA), which facilitates AR dissemination. However, recovery of exDNA from water samples is challenging. In this study, we validated a consecutive ultrafiltration-based protocol to simultaneously recover intracellular DNA (inDNA), dissolved exDNA (Dis_exDNA, dissolved in the bulk water), and adsorbed exDNA (Ads_exDNA, adsorbed to the surfaces of suspended particles). Using hollow fiber ultrafiltration (HFUF), all DNA fractions were concentrated from environmental water samples, after which Dis_exDNA (supernatant) was separated from inDNA and Ads_exDNA (pellets) using centrifugation. Ads_exDNA was washed off from the pellets with proteinase K and sodium phosphate buffer. Dis_exDNA and Ads_exDNA were further concentrated using centrifugal ultrafiltration, from which silica binding was performed. inDNA was extracted from washed pellets with a commercial kit. For inDNA, HFUF showed recovery efficiencies of 96.5 ± 18.5% and 88.0 ± 2.0% for total cells and cultured Escherichia coli, respectively (n = 3). To represent all possible DNA fragments in water environment, exDNA with different lengths (10.0, 4.0, 1.0, and 0.5 kbp) were spiked to test the recovery efficiencies for Dis_exDNA. The whole process achieved 62.2%–62.9% recovery for 10 and 4 kbp exDNA, and 38.8%–44.5% recovery for 1.0 and 0.5 kbp exDNA. Proteinase K treatment enhanced the recovery of Ads_exDNA by 4.0–10.7 times. The protocol was applied to water samples from an urban river in Tokyo, Japan. The abundance of AR genes (ARGs) in inDNA, Dis_exDNA, and Ads_exDNA increased downstream of wastewater treatment plants. ARGs in Ads_exDNA and Dis_exDNA accounted for 1.8%–26.7% and 0.03%–20.9%, respectively, of the total DNA, implying that Ads_exDNA and Dis_exDNA are nonnegligible potential pools for the horizontal transfer of ARGs.

The present work reported a high-throughput strategy for the analysis of 21 perfluorinated compounds (PFCs) in drinking water, tap water, river water and plant effluent from southern China by supramolecular solvent (SUPARS) vortex-mixed microextraction combined with high performance liquid chromatography-Orbitrap high resolution mass spectrometry (HPLC-Orbitrap HRMS). The SUPRAS without heating assistance is less solvent-consumption, meeting the requirements for green environmental protection and sustainable development. Parameters in the microextraction such as volume of dodecanol and tetrahydrofuran (THF), vortexing extraction and centrifugation time, salt concentration were investigated. The optimal extraction conditions were 250 μL of undecanol, 1.0 mL of THF and 20.0% (w/v, 4 g) NaCl. Under the optimum conditions, method limit of detection and method limit of quantitation in the ranges of 0.01–0.08 μg/L and 0.03–0.25 μg/L, good recoveries (72.5–117.8%) and intra-day precision (1.1–11.2%, n = 6), high enrichment factors (48–78) were obtained. The developed method was successfully applied for analysis of PFCs in 13 drinking water, tap water, river water and plant effluent samples collected from southern China. Perfluorobutane sulfonic acid was detected in one river water with concentration of 0.48 μg/L and 1H,1H,2H,2H-Perfluorooctane sulfonic acid was detected in one river water and two plant effluent samples with concentrations in the range of 0.14–0.67 μg/L.

The primary objective of this study was to identify the capacity and mechanism of extracellular polymeric substance (EPS) adsorption on soil colloids of Alfisol and Ultisol at different pH and ionic strengths. Two kinds of EPS were extracted from Bacillus subtilis and Pseudomonas fluorescens by centrifugation, and their adsorption on Ultisol and Alfisol was investigated using a batch adsorption experiment and attenuated total reflectance–Fourier transform infrared spectroscopy (ATR-FTIR). The average diameter of EPS from B. subtilis and P. fluorescens was 1825 and 1288 nm, respectively, and both the EPS were negatively charged. The zeta potentials of the two EPS became more negative with increasing solution pH from 3 to 8 and less negative with increasing ionic strength from 0 to 80 mM. The maximum adsorption capacity of EPS-C and EPS-N on Alfisol was higher than that on Ultisol, whereas the maximum adsorption capacity of EPS-P on Alfisol was lower than that on Ultisol. The adsorption of EPS-C, EPS-N, and EPS-P of both the EPS on Ultisol and Alfisol decreased with increasing solution pH from 3 to 8. Adsorption of EPS-C, EPS-N, and EPS-P of both the EPS on Alfisol significantly increased with increasing ionic strength from 0 to 10 mM, whereas it remained constant, slightly increased, or reduced, when the ionic strength was increased from 10 to 80 mM. The adsorption of EPS-C, EPS-N, and EPS-P on Ultisol slightly increased with increasing ionic strength from 0 to 80 mM. Saturation coverage determined by ATR-FTIR showed that adsorption of whole EPS on Ultisol was higher than that on Alfisol at pH 6 after 60 min. Thus, electrostatic force between EPS and soil colloids played an important role in EPS adsorption. Besides, proteins and phosphate groups in EPS also contributed to EPS adsorption on soil colloids.

The ubiquitous presence of microplastics (MPs) has been demonstrated in all environmental compartments in the recent years. They are detected in air, freshwater, soil, organisms and particularly in marine ecosystems. Since sediments are known to be the major sink of many organic and inorganic pollutants, the aim of this study was to develop and validate a fast and cheap methodology to assess the MP contamination in intertidal sediments from the Gulf of Biscay (Pays de la Loire region, France). Sediments were sampled at three locations (Pays de la Loire region, France) and during two seasons: October 2015 and March 2016. The analytical protocol involved MP extraction from dried sediments using milliQ water and a centrifugation technique. After a filtration step of supernatants, MPs were detected and directly identified on the membrane filters using μFTIR spectroscopy in reflection mode. For the first time, the number of replicates allowing to obtain a satisfying representativeness of the whole sampled sediment was also evaluated at 10 replicates of 25 g each. The average number of MPs in sediments was 67 (±76) MPs/kg dw (N = 60) with no significant difference between sites and seasons. Ten different compositions of MPs were defined by μFT-IR with a high proportion of polypropylene (PP) and polyethylene (PE), 38 and 24%, respectively. Among MPs, mainly fragments (84%) were observed with main size classes corresponding to [>100 μm] and [50–100 μm] but no particles > 1 mm could be found suggesting that mainly small microplastics (<1 mm) were subject to vertical transport.

Accurate quantification of nanoplastics (NPs) in complex matrices remains a challenge, especially for biological samples containing high content of organic matters. Herein, a new method extracting and quantifying polystyrene (PS) NPs from biological samples was developed. The extraction included alkaline digestion, centrifugation, and cloud point extraction (CPE), and the quantification included gold nanoparticles formation and labeling on surfaces of the extracted NPs and thereafter measurement with single particle inductively coupled plasma mass spectrometry (SP-ICP-MS). Results show that 25% tetramethylammonium hydroxide solution was an effective alkaline digestion solution for biological matrices, and CPE after centrifugation (3000 rpm, 10 min) was applicable to purify and enrich PS NPs with different sizes (100 and 500 nm) and surface functionalities (-COOH and –NH₂ modifications) from the digestion solution. The efficiency of Au labeling on PS NPs surface was improved by about 70% in the presence of 100 μM cetyltrimethylammonium bromide. The performance of the quantification method was examined by extraction and measurement of PS NPs spiked in four representative organism samples including bacteria, algae, nematode, and earthworm, and was further validated by analyzing the accumulated PS NPs in exposed nematodes. Good recovery rates (65 ± 10%–122 ± 22%) were achieved for spiking levels of 5–50 μg g⁻¹; the limit of detection was 3.7 × 10⁷ particles g⁻¹, corresponding to the mass concentration of about 0.02 and 2.5 μg g⁻¹ for the 100 nm and 500 nm PS NPs, respectively. The established extraction and quantification methods are efficient and sensitive, providing a useful approach for further exploring the environmental behavior and toxicity of NPs.

A microextraction method for the determination of triclosan and methyltriclosan in marine environmental samples was developed. The disperser was first serves as a preliminary extractant for analytes, then as a frozen solvent to remove impurities at −20 °C, and finally as a disperser agent in the microextraction procedure. With the extractants solidified and float on the surface of the aqueous phase at low temperature, a separation was achieved to avoided use of specialized laboratory instruments. The method was optimized using Plackett-Burman design and central composite design as follows: 146 μL octanoic acid as extractant, 793 μL acetoneas disperser, 3.0 min centrifugation and 1.1 min vortex time. The limits of detection were 0.022–0.060 μg L−1 or μg kg−1 and recoveries were 83.3–103.5% for TCS and MTCS in seawater, sediments and seafood. The method has excellent prospects for sample pre-treatment and trace-level analysis of triclosan and methyltriclosan in marine environmental samples.

As observed among residents in electronic waste (e-waste) recycling areas, dioxins can disrupt the homeostasis of endocrine hormones and the balance of thyroid hormones. Few studies, however, have examined whether e-waste recycling activities influence steroid hormone equilibrium in the general adult male population. This study evaluated the association between steroid hormones and the physical burdens of dioxins in the general adult male population residing in an e-waste region. In September 2017, 74 adult males residing in an e-waste dismantling region were enrolled in the current study. Approximately 10 mL of blood was collected from each adult male, and the serum samples were separated through centrifugation. Then, the levels of dioxin and steroid hormones in the serum of the participants were measured. We treated dioxin levels as categorical variables in the general linear model according to quartiles (25, 50, and 75 percentile). Comparing the findings with a reference group (< 25th percentile), we noted significantly higher dehydroepiandrosterone (DHEA) level in men with low serum polychlorinated dibenzofuran-toxic equivalent (PCDFs-TEQ) level between 3.80 and 6.31 pg/g lipid (1933 vs. 1447 pg/ml) and low polychlorinated dibenzo-p-dioxins and dibenzofurans-TEQ (PCDD/PCDFs-TEQ) between 8.57 and 15.11 pg/g lipid (1996 vs. 1360 pg/ml). Moreover, a significantly higher androstenedione (A-dione) level was found in men whose serum PCDFs-TEQ ≥ 11.34 pg/g lipd (2404 vs. 1848). What’s more, there were significantly higher 3β-hydroxysteroid dehydrogenase (3β-HSD) concentrations in low- and high-2,3,7,8-tetrachlorodibenzo-p-dioxin (TCDD) groups (1.30–1.67 and ≥ 2.64 pg-TEQ/g lipid, respectively with 719 and 807 vs. 496, respectively). Our findings suggest that specific dioxin exposure may disturb normal DHEA, A-dione levels, and enzyme activity in the general adult male population in an e-waste region of China.

The mechanisms by which complex products released from the organic matrix of cattle manure impact phosphorus (P) behavior and transport are largely undefined. Effects of a dairy slurry isolate on sorption characteristics of three benchmark soils and the breakthrough of phytate-P were determined in short soil columns of Mattapex loam (fine-silty, mixed, active, mesic Aquic Hapludults) under saturated flow conditions. The manure liquid isolate was obtained after a 7-day incubation of reconstituted dairy manure (1.6:1, feces-to-urine) at 37 °C and centrifugation at 16,000×g. The liquid isolate, at dilutions of 20:1 to 4:1 water-to-isolate, decreased soil sorption of phytate-P, with reduction in logₑ K averaging 30%. Whether the influent contained artificial rainwater or the manure isolate at a water-to-isolate ratio of 20:1, P retention and breakthrough curves were differentially impacted. Only inorganic phosphate-P was eluted in a multiple-stage process, and breakthrough occurred after 16 pore volumes of rainwater. Both inorganic- and enzyme-labile P (TBIOP) appeared in the effluent when either a dilute solution of 0.05 M EDTA (ethylenediamine-N, N, N′, N′-tetraacetate) or one containing 5% of manure liquid isolate was used as influent. The polydentate ligand-like substances reduced (i) the soil’s affinity for phytate and (ii) the hydrolysis rate in soil, allowing phytate to be eluted. Therefore, dissolved components of the manure matrix played critical roles in controlling transport and dispersion of phytate-derived P forms in soil and may hold the key to the understanding of biogeochemical bases of persistent effects of legacy P in agricultural watersheds.

In this work, we developed a method based on ultrasound-assisted emulsification microextraction (USAEME) for the determination of nickel by flame atomic absorption spectrometry (FAAS). The method is based on the use of the organic solvent trichloroethylene and 2,2′-thiazolylazo-p-cresol (TAC) as a chelating reagent in a solution containing nickel ions. After ultrasonic emulsification, the mixture is centrifuged to separate the phases. Subsequently, the supernatant is discarded, and the enriched phase is diluted with nitric acid. The nickel content in this new mixture is quantified by FAAS. The following variables were optimized: type of solvent (trichloroethylene), type of chelating reagent (TAC), volume of extraction solvent (100 mL), concentration of chelating reagent (0.015 % w/v), pH (8.0), time of sonication (5.0 min), and time of centrifugation (4.0 min). The limits of detection and quantification were calculated under optimum conditions (0.23 and 0.77 μg L⁻¹, respectively). The enrichment factor obtained was 190. The relative standard deviation (RSD%) of the method (10.0 μg L⁻¹) was 2.3–4.1 %. The proposed method is simple, economical, fast, and efficient for the determination of nickel by FAAS. The procedure was applied to the determination of nickel in certified reference material (BCR-713, wastewater) and water samples.

Despite all its advantages and potential, cross-linking enzyme aggregate (CLEA) technology is still not applied at an industrial scale for enzyme insolubilization for bioremediation purposes. In this study, the enzyme polymer engineered structure (EPES) method was used to enhance CLEA stability and reuse. A crude laccase from Trametes hirsuta was successfully insolubilized to form EPES-CLEAs. The polymeric network provided excellent stability (> 90%) to CLEAs after a 24-h incubation in a non-buffered municipal wastewater effluent (WW), and the biocatalysts were recycled using a centrifugation process. While CLEAs activity dropped to 17%, EPES-CLEAs showed a laccase activity retention of 67% after five cycles of 2,2’-azino-bis (3-ethylbenzthiazoline-6-sulfonic acid) (ABTS) oxidation. After 8 h of treatment in WW, the EPES-CLEAs were equally as effective in removing cannabidiol (CBD) as the free-LAC (~ 37%). This research demonstrates that the EPES method is a promising alternative for CLEA stabilization and reuse in environmental conditions.