BACKGROUND: Concentrations of metoprolol in exhaled breath condensate (EBC) have not been investigated. Herein, we aim to determine the metoprolol levels in EBC, plasma, and urine samples.
METHODS: Biological samples were collected from 39 patients receiving metoprolol. Metoprolol was determined using liquid chromatography mass spectrometery. The obtained metoprolol levels in biological fluids were investigated for possible inter-correlations.
RESULTS: Acceptable linearity was obtained with coefficient of determinations equal to 0.9998, 0.9941, and 0.9963 for EBC, plasma, and urine samples, respectively. The calibration curves were linear in the ranges of 0.6-500, 0.4-500, and 0.7-10,000 µg·L- 1 regarding EBC, plasma, and urine samples, respectively. The detection and quantification limits were (0.18, 0.12, and 0.21 µg·L- 1) and (0.60, 0.40, and 0.70 µg·L- 1) for EBC, plasma, and urine samples, respectively. The relative standard deviations for the intra- and inter-day replications were obtained between 5.2 and 6.1 and 3.3-4.6%, respectively. The obtained mean metoprolol levels in EBC, plasma, and urine samples of 39 patients were 5.35, 70.76, and 1943.1 µg·L- 1. There were correlations between daily dose and plasma and urinary concentrations of metoprolol in the investigated samples, whereas no significant correlation was observed for daily dose and EBC levels. The correlation among plasma-urine levels was significant, however, the non-significant correlation was obtained between plasma and EBC concentrations.
CONCLUSIONS: Metoprolol levels varied widely due to the metabolic pattern of the Azeri population, different dosages received by the patients, formulation effects, age, sex, and interactions with the co-administered drugs. A poor correlation of EBC-plasma concentrations and a significant correlation of plasma-urine concentrations were observed. Further investigations are required to provide the updated services to personalized medicine departments.

Severe acute respiratory syndrome coronaviruses 2 (SARS-CoV-2) causing coronavirus disease 2019 (COVID-19) affected the health of human beings and the global economy. The patients with SARS-CoV-2 infection had viral RNA or live infectious viruses in feces. Thus, the possible transmission of SARS-CoV-2 through wastewater received great attentions. Moreover, SARS-CoV-2 in wastewater can serve as an early indicator of the infection within communities. We summarized the preconcentration and detection technology of SARS-CoV-2 in wastewater aiming at the complex matrices of wastewater and low virus concentration and compared their performance characteristics. We described the emerging tests that would be possible to realize the rapid detection of SARS-CoV-2 in fields and encourage academics to advance their technologies beyond conception. We concluded with a brief discussion on the outlook for integrating preconcentration and the detection of SARS-CoV-2 with emerging technologies.

A new, simple and rapid spectrophotometric method was developed for determination of Sudan Black B in food products by supramolecular solvent-based-vortex-assisted-dispersive liquid liquid microextraction (SUPRAS-VA-DLLME). Extraction solvent type, volume of solvent, pH, volume of THF, centrifugation time, vortex time, and sample volume were investigated as optimization parameters of the developed method. Under the optimum conditions, limit of detection and limit of quantification, preconcentration factor and enhancement factor of the developed method were calculated to be 9.01 μg L-1, 29.73 μg L-1, 20, and 55, respectively. The developed microextraction method was successfully applied to food samples for the determination of Sudan Black B.

Microplastics is known to be ubiquitous in aquatic environment. Quantification of microplastics in natural waters is an important problem of analytical chemistry, the solution of which is needed for the assessment of water quality and potential risks for water inhabitants and consumers. Separation methods play a key role in the correct quantification of microplastics in natural waters. In the present study the applicability of countercurrent chromatography to the continuous-flow separation and preconcentration of microplastics from water samples in rotating coiled column (RCC) using water-oil systems has been demonstrated for the first time. The effect of column rotation speed and mobile phase (water) flow rate on the retention of the stationary (oil) phase in RCC is studied. The retention parameters of 10 vegetable and 2 synthetic oils are determined. Castor, olive, rapeseed, soybean, linseed, sesame, and sunflower oils are found to be applicable to the separation of microplastics from water samples using RCC. Taking as example polyethylene microparticles of different size (40-63, 63-100, and 100-250 μm), the high recovery of microplastics (about 100 %) from aqueous phase into castor and rapeseed oils is shown. The method has been proven to be efficient for the separation of microplastics from simulated fresh and sea natural waters. It may be perspective not only for the quantification of microplastics in natural waters but as well as for the purification of wastewaters containing microplastics.

A novel cloud-point extraction (CPE) procedure for the determination of ultra-trace amounts of arsenic species in real samples, purchased from the local market by spectrophotometer was developed. Inorganic arsenic species analysis in water, beverages, and foods has become increasingly important in recent years, as arsenic species are considered carcinogenic and are assessed at significant levels in samples. The technique is established on a selective ternary complex of As(V) with astrazon orange G (AOG+) in the presence of tartaric acid and polyethylene glycol tertoctylphenyl ether (Triton X-114) at pH 4.0. The calibration curve developed within range 3.0-160 ng/mL with a correlation coefficient of 0.9988 for As(V) provided a preconcentration factor of 200 and a limit of detection (3S blank/m) of 0.88 ng/mL under optimum investigation conditions. The results of molar absorptivity and Sandell sensitivity are calculated and found to be 4.38 × 105 L/mol cm and 0.018 ng cm-2, respectively. The statistical treatment of data obtained from the proposed and GF-AAS procedures are compared in terms of Student\'s t-tests and variance ratio F-tests has revealed no significant differences. The methodology has been effectively confirmed by assessing real samples and comparing it to the GF-AAS method statistically.

This work explores strategies for electrokinetic preconcentration of extracellular vesicles (EVs) that are potential source of biomarkers for different diseases. The first approach that led to successful preconcentration of EVs is based on large volume sample stacking (LVSS), allowing an enrichment factor of 7 for CE of EVs with long-end injection (using a capillary with an effective length of 50 cm). Attempts were also made to perform multiple cycles of LVSS, field amplified sample stacking (FASS) and field amplified sample injection (FASI), to improve EVs preconcentration performance. The focus was then put on development of capillary isotachophoresis under high ionic strengths (IS) for electrokinetic enrichment of slow migrating EVs having heterogeneous mobilities. This approach relies on the use of extremely high concentrations of the terminating electrolyte (TE) to slow down the mobility of TE co-ions, rendering them slower than those of EVs. The limit of detection for intact EVs using the developed ITP-UV method reached 8.3 × 108 EVs/mL, allowing an enrichment of 25 folds and a linear calibration up to 4 × 1010 EVs/mL. The ITP-UV and ITP-LIF approaches were applied to provide the electrokinetic signature of EVs of bovine milk and human plasma as well as to visualize more specifically intravesicular fluorescently labelled EVs. The investigation of these strategies shredded light into the challenges still encountered with electrokinetic preconcentration and separation of heterogeneous EVs sub-populations which are discussed herein based on our results and other attempts reported in the literature.

In the era of liquid biopsy, microRNAs emerge as promising candidates for the early diagnosis and prognosis of cancer, offering valuable insights into the disease\'s development. Among all the existing analytical approaches, even if traditional approaches such as the nucleic acid amplification ones have the advantages to be highly sensitive, they cannot be used at the point-of-care, while sensors might be poorly sensitive despite their portability. In order to improve the analytical performance of existing electroanalytical systems, we demonstrate how a simple chromatographic paper-based disk might be useful to rationally improve the sensitivity, depending on the number of preconcentration cycles. A paper-based electrochemical platform for miRNA detection has been developed by modifying a paper-based electrode with a methylene blue (MB)-modified single-stranded sequence (ssDNA) complementary to the chosen miRNA, namely miR-224 that is associated with lung cancer. A detection limit of ca. 0.6 nM has been obtained in spiked human serum samples. To further enhance the sensitivity, an external chromatographic wax-patterned paper-based disk has been adopted to preconcentrate the sample, and this has been demonstrated both in standard and in serum solutions. For each solution, three miR-224 levels have been preconcentrated, obtaining a satisfactory lowering detection limit of ca. 50 pM using a simple and sustainable procedure. This approach opens wide possibilities in the field of analytical and bioanalytical chemistry, being useful not only for electrochemistry but also for other architectures of detection and transduction.

BACKGROUND: Cyanide anion can be found in foodstuffs, tobacco smoke and a variety of types of waters, mainly originating from anthropogenic activities. Due to its highly toxic nature, several agencies have established limits for cyanide levels in water. Additionally, monitoring cyanide levels in biological samples, such as blood and urine, is crucial for obtaining clinical information about the health condition of patients. Therefore, there is a pressing need for the development of simple, cost-effective, and reliable analytical methods capable of quantifying cyanide at low concentrations.
RESULTS: This study presents a novel analytical method for the selective and sensitive determination of cyanide based on analyte volatilization, pre-concentration via single-drop microextraction (SDME) using a selective reagent, and colorimetric quantification using a paper-based analytical device. For this, 10 mL of a liquid sample was acidified with phosphoric acid and the generated HCN was collected using a single drop of 3 μL of a palladium dimethylglyoximate solution (Pd (DMG)22-) positioned in the flask headspace using a syringe. The reaction of Pd (DMG)22- leads to the formation of Pd(CN)42- and the demasking of the organic ligand. After 15 min of extraction time, the reagent drop was added to a paper-based analytical device that has been previously impregnated with 3 μL of nickel chloride, resulting in the formation of a red precipitate of nickel (II) dimethylglyoximate. Digital images of the paper-based device were captured and the red channel (R) was used for quantification purposes. Under optimized conditions, the method demonstrates a suitable linear relation (r2 > 0.99) ranging from 26 to 286 μg L-1 and a limit of detection of 5 μg L-1.
CONCLUSIONS: As a proof of concept, cyanide levels were quantified in water and urine samples using this method. The proposed approach offers high sensitivity and selectivity while requiring only a small volume of reagents. Furthermore, it exhibits a high degree of portability for in-situ applications.

A new magnetic nano gel (MNG) was prepared from choline chloride/phenol deep eutectic solvent and magnetic amberlite XAD-7 nanocomposite. The dispersive solid phase micro extraction (dSPME) method was developed for seperation and preconcentration of Brilliant Blue FCF (BB) by the prepared MNG. In this study, firstly, the optimum DES type and mole ratio of DES were investigated before response surface methodology optimization. Then, the effect of the MNG-dSPME experimental parameters were optimized by response surface methodology using central composite design. Under the optimum microextraction conditions, limit of detection (LOD), limit of quantification (LOQ), preconcentration factor (PF), enhencament factor (EF) were found to be 1.15 μg L-1,3.80 µg L-1, 70, and 88, respectively. It was seen that the recovery of real samples were obtained from 95.5 to 103.6%. The pesent method was succesfully for extraction of BB in some food, personal care samples, to the best of our knowledge, this is the first study that is presented method on determination of BB by preconcentration with magnetic nano gel. The obtained results showed that the present procedure is effective, sensitive, and has high accuracy for the quantitative detection of BB.

In this research, a new approach based on magnetic electrodes has been developed for the determination of per-fluorooctane sulfonic acid (PSOF). Zinc and Titanium-based Metal-organic framework (MOF) was synthesized and used with polypyrrole as a conductive polymer for preparation of the absorbent to achieve the best performance for electrochemical application. The response of the electrode for determination of the PFOS was affected and optimized by different factors such as buffer solution, pH of the solution, amount of absorbent, extraction time of absorbent, accumulation time, as well as the Square Wave Voltammetry (SWV) instrumental parameters including voltage step, pulse amplitude, frequency and resting time. In the optimum condition, the response of the Zn/Ti/C-MOF-magnetic molecular imprinting polymer/carbon paste electrode (MOFMMIP/CPE) has increased logarithmically by increasing the concentration in the range of 0.002-165 μM by the limit of detection (LOD) of 0.7 nM. The obtained percentage of Recovery (96.00-104.14 %), Bias (-4.00 - 4.14 %) and Relative Standard Deviation (RSD) (1.89-3.74 %) for determination of the PFOS in real and spiked tap water, river water and well water samples demonstrates that the proposed method has an acceptable precision. The comparison between the gained data by the presented method and High-performance liquid chromatography (HPLC) showed that the presented method has high accuracy.