Electroextraction of methylene blue from aqueous environmental samples using paper points coupled with hollow fiber membranes.

This article introduces a novel approach by coupling paper points with hollow fiber membrane for electroextraction (PP-HF-EE). The method was innovatively applied to extract methylene blue (MB) from large water volumes (up to 580 mL). A comprehensive study of six key parameters - organic filter, acceptor and donor phase composition, extraction time, applied voltage, and sample volume - was conducted using conventional flatbed scanning and digital image analysis. Our results revealed that extraction performance was primarily influenced by time, with low voltages (50 V) and low-conductivity organic filters (1-decanol) yielding comparable results to higher settings (300 V or 1-pentanol). Under optimized conditions (50 V, 60 min, 1-decanol as the organic filter), analytical performance parameters were assessed, demonstrating acceptable precision (RSD <18% for intra- and inter-day measurements) within a linear range of 5-100 µg L-1 (r = 0.98). PP-HF-EE demonstrated reliability through stable and reproducible electric current measurements during all extraction studies. Utilizing an extremely cost-effective detection system, PP-HF-EE achieved detection limits in the low ppb range, highlighting its potential as a promising variation of electromembrane extraction for environmental sample analysis.

Layer-by-layer assembly of PDDA/MWCNTs thin films as an efficient strategy for extraction of organic compounds from complex samples.

This article presents the assembly and characterization of poly(diallyldimethylammonium chloride)/multi-walled carbon nanotubes (PDDA/MWCNTs) thin films on borosilicate bottles using a layer-by-layer (LBL) approach. The thin films, consisting of 10 bilayers of coating materials, were thoroughly characterized using UV-VIS spectroscopy, scanning electron microscopy (SEM), and zeta potential measurements. The modified bottles were then utilized for the extraction of analytes with diverse acid-base characteristics, including drugs, illicit drugs, and pesticides, from saliva, urine, and surface water samples. The studied analytes can be adsorbed on the surface of the LBL film mainly through hydrogen bonding and/or hydrophobic interactions. Remarkably high extraction percentages of up to 92 % were achieved, accompanied by an impressive enhancement in the analytical signal of up to 12 times when the sample volume was increased from 0.7 to 10 mL. These results highlight the outstanding extraction and sorption capabilities of the developed material. Additionally, the (PDDA/MWCNTs)10 films exhibited notable resistance to extraction and desorption processes, enabling their reuse for at least 5 cycles. The straightforward and cost-effective fabrication of these sorbent materials using the LBL technique, combined with the ability to extract target compounds during sample transportation and/or storage, renders this sample preparation method a promising alternative.

The Antimicrobial Applications of Nanoparticles in Veterinary Medicine: A Comprehensive Review.

Nanoparticles (NPs) are nanoscaled particles sized from 1-100 nm, which can be composed of inorganic or organic compounds. NPs have distinctive morphology, size, structure, and surface features, which give them specific properties. These particular attributes make them interesting for biological and medical applications. Due to these characteristics, researchers are studying the possible aptness of numerous nanoparticles in veterinary medicine, such as the capacity to act as a drug delivery system. The use of these NPs as a possible bactericidal or bacteriostatic medication has been studied against different bacteria, especially multiresistant strains and the ones that cause mastitis disease. The antibiofilm property of these nanostructures has also already been proved. The antiviral activity has also been shown for some important viral animal diseases; the antifungal activity had been demonstrated against both pathogenic and mycotoxigenic species. Therefore, this review aimed to elucidate the main clinical and preventive veterinary applications of inorganic and organic nanoparticles.

Direct coupling of paper spray mass spectrometry and four-phase electroextraction sample preparation.

This paper presents a novel coupling between a four-phase electroextraction (EE) system and paper spray mass spectrometry (PS-MS) for the extraction, pre-concentration, and direct analysis of target compounds in different samples. The approach, EE-PS-MS, is based on the sorption of analytes directly on the tip of a triangular-shaped chromatographic paper, with subsequent prompt analysis by PS-MS. Thus, no off-line extraction step is required before the PS analysis, improving the protocol efficiency and reducing the analysis time. In addition to functioning as a porous material to absorb the target compounds, the chromatographic paper also served as the support for one of the aqueous phases of the optimized four-phase electroextraction system. Extraction conditions, such as the composition of the donor and organic phases, applied electric potential, and extraction time, were optimized. Three different applications, involving biofluid, food, and water quality analysis, were evaluated as a proof-of-concept. These applications involved the determination of (i) cocaine and lidocaine in saliva, (ii) malachite green in tap water, and (iii) bisphenol A (BPA) in red wine. When compared with direct PS-MS, the novel EE-PS-MS protocol improved the sensitivities by factors ranging from 14 to 110, depending on the analyte and the sample. The electroextraction procedures were performed on a laboratory-built 66-well plate, which offered the functionality of simultaneous sample handling and, most importantly, improved analytical throughput.

Electric field-assisted multiphase extraction to increase selectivity and sensitivity in liquid chromatography-mass spectrometry and paper spray mass spectrometry.

In this work, for the first time, chromatographic paper was used for a multiphase extraction assisted by an electric field (MPEF) and directly coupled to paper spray mass spectrometry (PS-MS). Using this approach, five tricyclic antidepressants (TCAs) were determined in oral fluid. Firstly, the MPEF conditions were optimized using liquid chromatography-mass spectrometry (LC-MS/MS). The effects of the chromatographic paper and the types of electrolyte used in the acceptor phase, the organic solvent type and the amount used in the donor phase, the extraction time, and the applied electric potential were all investigated. After optimization, the analytes were extracted from the donor solution (sample and acetonitrile 1:1 (v/v)) over a period of 10 min at 300 V, crossing the free liquid membrane (1-octanol) and reaching the acceptor phase (chromatographic paper wetted with 400 mmol L-1 acetic acid). The method using LC-MS/MS was validated, demonstrating a linear range from 2 to 12 ng mL-1, with detection and quantification limits of 0.13-0.25 and 0.44-0.84 ng mL-1, respectively, an intraday precision of less than 20%, and no matrix effect observed. The optimized MPEF conditions were then applied to determine TCAs by PS-MS and for this analysis cyclobenzaprine was used as an internal standard. The easy, fast and direct approach of coupling MPEF with PS-MS analysis, as well as the pre-concentration and the low standard deviation of replicates (less than 20%), demonstrates that this method can be useful for screening in clinical and toxicological analysis.

Development and Evaluation of a 66-Well Plate Using a Porous Sorbent in a Four-Phase Extraction Assisted by Electric Field Approach.

In this work, cellulose cone tips were used as a hydrophilic sorbent supporting an aqueous electrolyte solution in a four-phase electric-field-assisted extraction. The wetted tips were immersed in an immiscible organic phase, acting as a filter to extract analytes present in an aqueous sample. Simultaneous four-phase extractions were carried out under the influence of an electric field using a 66-well plate constructed with inexpensive and readily available laboratory materials. Several parameters that control the electric resistivity of the system were evaluated, and the cone tips provided reproducible and stable electric current during application of electric potential difference. In a final application, a cationic dye and its metabolite, crystal and leuco crystal violet, were extracted from spiked fish extracts and quantified by a digital image analysis method. The method presented a linear range of 2-100 ng mL-1 ( r > 0.999), limit of detection of 1.37 ng mL-1, inter- (3 consecutive days) and intraday precision determined for 4 concentration levels ( n = 6, each) were lower than 29% and mean recoveries for these concentrations ranging from 95% to 115%. The results demonstrated that the 66-well plate provides a stable, reproducible, and simple way to conduct extractions of ionic compounds from complex aqueous matrixes. The effectiveness of the low-cost cellulose cone tips used as a solid fourth phase also confirmed that it can easily overcome many drawbacks of similar liquid-liquid-liquid approaches.

Simultaneous determination of fumonisins B1 and B2 in different types of maize by matrix solid phase dispersion and HPLC-MS/MS.

This work involved the optimization and validation of a method, according to Directive 2002/657/EC and the Analytical Quality Assurance Manual of Ministério da Agricultura, Pecuária e Abastecimento, Brazil, for simultaneous extraction and determination of fumonisins B1 and B2 in maize. The extraction procedure was based on a matrix solid phase dispersion approach, the optimization of which employed a sequence of different factorial designs. A liquid chromatography-tandem mass spectrometry method was developed for determining these analytes using the selected reaction monitoring mode. The optimized method employed only 1g of silica gel for dispersion and elution with 70% ammonium formate aqueous buffer (50mmolL-1, pH 9), representing a simple, cheap and chemically friendly sample preparation method. Trueness (recoveries: 86-106%), precision (RSD ≤19%), decision limits, detection capabilities and measurement uncertainties were calculated for the validated method. The method scope was expanded to popcorn kernels, white maize kernels and yellow maize grits.

Electrical field assisted matrix solid phase dispersion as a powerful tool to improve the extraction efficiency and clean-up of fluoroquinolones in bovine milk.

This work presents a new method by electrical matrix solid phase dispersion for the extraction and clean-up of marbofloxacin, ofloxacin, norfloxacin, ciprofloxacin, enrofloxacin, difloxacin and sarafloxacin in bovine milk. Composition and pH of the eluent, applied electrical potential and polarity were optimized by experimental designs. The combination of the chromatographic and electrophoretic mechanisms allowed the extraction and clean-up in one step with low organic solvent consumption, high extraction throughput and elution automation. Linearity, precision, trueness and limit of quantification were evaluated and provided values in accordance with other methods recently developed for the analysis of fluoroquinolones in milk. This technique proved to be promising for the extraction and clean-up of ionizable analytes in different milk matrices.

Electric field-assisted solid phase extraction and cleanup of ionic compounds in complex food matrices: Fluoroquinolones in eggs.

The use of electric fields as additional driving forces in sample preparation techniques is an innovative approach that is environmentally friendly, straightforward, and able to overcome several limitations of conventional sample preparation procedures. In this work, the advantages of electric field-assisted solid phase extraction (E-SPE) using syringe-type cartridges were demonstrated for the extraction of four fluoroquinolones (FQs) in their anionic forms. The FQs were extracted from eggs and subsequently determined by UHPLC-MS/MS. The use of electric fields during the washing and final elution steps resulted in a significant improvement of the extraction efficiencies for almost all FQs when compared to conventional SPE. Intra- and inter-day assays showed coefficients of variation below 10%. The better cleanup also resulted in the appearance of less precipitated matter in the final eluate, as well as reduced matrix effects. The results showed that the electrophoretic forces derived from electric fields are a promising way of significantly increasing the extraction efficiency of ionic analytes, while minimizing matrix effects associated with complex samples.

Simple and efficient method for enantioselective determination of omeprazole in human plasma.

A practical and selective HPLC method for the separation and quantification of omeprazole enantiomers in human plasma is presented. C18 solid phase extraction (SPE) cartridges were used to extract the enantiomers from plasma samples and the chiral separation was carried out on a Chiralpak AD column protected with a CN guard column, using ethanol:hexane (70:30) as the mobile phase, at a flow rate of 0.5 ml/min. The detection was carried out at 302 nm. The method proved to be linear in the range of 10-1000 ng/ml for each enantiomer, with a quantification limit of 5 ng/ml. Precision and accuracy, demonstrated by within-day and between-day assays, were lower than 10%.