Use of nanomaterials in the pretreatment of water samples for environmental analysis

The challenge of providing clean drinking water is of enormous relevance in today’s human civilization, being essential for human consumption, but also for agriculture, livestock and several industrial applications. In addition to remediation strategies, the accurate monitoring of pollutants in water sup-plies, which most of the times are present at low concentrations, is a critical challenge. The usual low concentration of target analytes, the presence of in-terferents and the incompatibility of the sample matrix with instrumental techniques and detectors are the main reasons that renders sample preparation a relevant part of environmental monitoring strategies. The discovery and ap-plication of new nanomaterials allowed improvements on the pretreatment of water samples, with benefits in terms of speed, reliability and sensitivity in analysis. In this chapter, the use of nanomaterials in solid-phase extraction (SPE) protocols for water samples pretreatment for environmental monitoring is addressed. The most used nanomaterials, including metallic nanoparticles, metal organic frameworks, molecularly imprinted polymers, carbon-based nanomaterials, silica-based nanoparticles and nanocomposites are described, and their applications and advantages overviewed. Main gaps are identified and new directions on the field are suggested.publishe

Salting-out assisted liquid–liquid extraction for the determination of ciprofloxacin residues in water samples by high performance liquid chromatography–diode array detector

Abstract Background The occurrence of emerging pollutants like pharmaceuticals and related compounds in the aquatic and terrestrial environments is of increasing concern. Ciprofloxacin is one of the pharmaceuticals which is active against a wide range of bacteria. The main objective of this research is to develop a simple method for the extraction and determination of ciprofloxacin residues in environmental water samples. Results A salting-out assisted liquid–liquid extraction (SALLE) method for the determination of ciprofloxacin in water samples by high-performance liquid chromatography with diode array detector (HPLC–DAD) was developed. The calibration curve was linear over the range of 0.1–100 μg/L with coefficient of determination (r2) of 0.9976. The limits of detection (LOD) and quantification (LOQ) of the method were 0.075 and 0.25 µg/L, respectively. The reproducibility in terms of relative standard deviation (% RSD) was less than 10%. The applicability of the developed method was investigated by analyzing tap water, bottled mineral water and waste water and demonstrated satisfactory recoveries in the ranges of 86.4–120%. Conclusion The method offered a number of features including wide linear range, good recovery, short analysis time, simple operation process and environmental friendly. The developed method can be utilized as an attractive alternative for the determination of ciprofloxacin residues in environmental water matrices

An integrated approach for trace detection of pollutants in water using polyelectrolyte functionalized magneto-plasmonic nanosorbents

Resistance of pathogenic micro-organisms to conventional antibiotics is an essential issue for public health. The presence of such pharmaceuticals in aquatic ecosystems has been of major concern for which remediation and ultra-sensitive monitoring methods have been proposed. A less explored strategy involves the application of multifunctional nanosorbents for the uptake and subsequent detection of vestigial contaminants. In this study, colloidal nanoparticles (NPs) of iron oxide and gold were encapsulated in multi-layers of a charged polyelectrolyte (PEI: polyethyleneimine), envisaging the effective capture of tetracycline (TC) and its subsequent detection by Surface Enhanced Raman Scattering (SERS). Adsorption studies were performed by varying operational parameters, such as the solution pH and contact time, in order to evaluate the performance of the nanosorbents for the uptake of TC from water. While the magnetic nanosorbents with an external PEI layer (Fe3O4@PEI and Fe3O4@PEI-Au@PEI particles) have shown better uptake efficiency for TC, these materials showed less SERS sensitivity than the Fe3O4@PEI- Au nanosorbents, whose SERS sensitivity for TC in water has reached the limit of detection of 10 nM. Thus, this study highlights the potential of such magneto-plasmonic nanosorbents as multi-functional platforms for targeting specific contaminants in water, by taking into consideration both functionalities investigated: the removal by adsorption and the SERS detection across the nanosorbents' surfaces.publishe