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N-Triflination associated with pyrazolones: a brand new way of N-S bond formation.
The proposed procedure proved to be fast (10 min), simple (two stages), inexpensive (10 mg of nanoparticles) and was applied to human serum samples. Unlike previously synthesized nanoparticles for tetracyclines separation, the surfactant-coated Fe3O4 nanoparticles can be easily prepared with widely available and low-cost reagents. Moreover, elution of the analytes was accomplished in absence of organic solvents by an aqueous chelating agent solution. As non-invasive biomarkers, exosomes are of great significance to diseases diagnosis. However, sensitive and accurate detection of exosomes still remains technical challenges. Herein, inspired by nature's "one-to-many" concept, we design a biosensor mimicking the cactus with numerous thorns to detect exosomes. The biosensor is composed of CD63 antibodies, resembling the roots of cactus, to capture exosomes, and the exosomes resemble the stems. Cholesterol-labeled DNA (DNA anchor) binding to streptavidin modified horseradish peroxidase (HRP) can insert into exosomes membrane, which seems the thorns. The readout signal is produced through HRP-catalyzed hydrogen peroxide (H2O2) mediated oxidation of 1,4-phenylenediamine (PPD) to form 2,5-diamino-NN'-bis-(p-aminophenyl)-1,4-benzoquinone di-imine (PPDox). The PPDox can quench fluorescence of fluorescein through inner filter effect (IFE), which provides fluorescent signal for exosomes detection. Based on this principle, the obtained exosomes solution is qualitatively and quantitatively analyzed by our biosensor, with the comparison to current standard methods by nanoparticle tracking analysis (NTA) and commercial enzyme-linked immunosorbent assay (ELISA) kit. The linear range is from 1.0 × 104 to 5.0 × 105 particles μL-1 with the limit of detection 3.40 × 103 particles μL-1 and 3.12 × 103 particles μL-1 for colorimetric and fluorescent assays, respectively. Meanwhile, our biosensor exhibits good selectivity, and can eliminate the interference from proteins. This dual-modal biosensor shows favorable performance towards analytical application in clinic samples, pushing one step further towards practical clinical use. An optical immunosensor based on White Light Reflectance Spectroscopy is described for the determination of the herbicide glyphosate in drinking water samples. The biosensor allows for the label-free real-time monitoring of biomolecular interactions taking place onto a SiO2/Si chip by transforming the shift in the reflected interference spectrum caused by the immunoreaction to effective biomolecular adlayer thickness. Glyphosate determination is accomplished by functionalizing the chip with a protein conjugate of the herbicide followed by a competitive immunoassay format. Prior to the assay, glyphosate derivatization in the calibrators and/or the samples was performed through reaction with succinic anhydride. Under the optimized assay protocol, a detection limit of 10 pg mL-1 was achieved. Recovery values ranging from 90.0 to 110% were determined in spiked bottled and tap water samples, demonstrating the accuracy of the method. In addition, the sensor could be regenerated and re-used for at least 14 times without statistically significant effect on the assay sensitivity and accuracy. The excellent analytical performance and short analysis time (approx. 25 min), combined with the small sensor size, should be helpful for the fast on-site determination of glyphosate in drinking water samples. This article reports on the development and validation of a disposable microfluidic paper-based analytical device (μPAD) for on-hand, in-situ, and cheap Fe(III) determination in natural waters complying with World Health Organization guidelines. The developed μPAD used 3-hydroxy-4-pyridinone (3,4-HPO) as a colour reagent due to its considerably lower toxicity than traditionally used iron analytical reagents. It was selected among a group of hydrophilic 3,4-HPO chelators containing ether-derived chains in their structure which were prepared using green methods. The relatively high water solubility of these chelators improved the detection limit and applicability as μPAD reagents. Under optimal conditions, the μPAD is characterised by a quantification range between 0.25 and 2.0 mg/L, a detection limit of 55 μg/L and 15 min of analysis time. The signal stability extends up to 4 h and the device is stable for at least one month. The reagent consumption is below 0.2 mg per analysis and the μPAD method was validated by analysis certified reference materials and by comparison with atomic absorption results (RD less then 10%). The newly developed μPAD was successfully applied to the determination of iron in river, well and tap waters with no need of any prior sample pre-treatment. A tailor-made diffusive sampler has been developed for the determination of nitrogen dioxide (NO2), sulfur dioxide (SO2) and ozone (O3) concentrations with a performance evaluation of the sampler being carried out under field and laboratory conditions. The most important characteristics of the sampler design is that simultaneous sampling of the three pollutants can be performed in one sampler. click here All the parts of the diffusive sampler are reusable after cleaning. These properties provide important advantages in terms of cost and practicality. Two alternative samplers, having long and short diffusion paths, have been designed. Extensive validation studies, including detection limit, precision, accuracy, recovery, shelf life, storage stability, comparison with commercial diffusive samplers, and the effects of shelter use were conducted in accordance with European Standards (EN). According to the validation results, all of the parameters evaluated for the diffusive sampler (for both long and short diffusion path designs) comply with the related standards and the sampler is expected to play an important role in the widespread monitoring of inorganic pollutants, since it is cheap, easy to use and deliverable within the country. In this work, Fe3O4/N co-doped hollow carbon spheres (Fe3O4@NHCS) as a promising electrocatalysis material had been prepared through carbonizing covalent organic frameworks and ferric irons. The morphology, structure, composition and electrocatalytic performance of Fe3O4@NHCS were characterized by various techniques. The electrode modified with Fe3O4@NHCS (Fe3O4@NHCS/GCE) exhibited excellent electrocatalytic activity for the oxidation of dopamine, uric acid, guanine and adenine. Simultaneous determination of these biomolecules was successfully achieved with Fe3O4@NHCS/GCE. Under the optimum conditions, the linear ranges for the determination of dopamine, uric acid, guanine and adenine were 0.01-40, 0.10-40, 0.50-30 and 0.50-40 μmol/L with the correlation coefficients of 0.9905, 0.9906, 0.9919 and 0.9908, respectively. The detection limits were 6.3, 36.1, 143.2 and 123.5 nmol/L for dopamine, uric acid, guanine and adenine, respectively (S/N = 3). In addition, the modified electrode was also applied to the simultaneous determination of these biomolecules in human serum samples and the recovery were varied from 97.
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