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Abstract Dimethyl 2-[2-(1-phenyl-4,5-dihydro-1H-imidazol-2-yl)hydrazinylidene]butanedioate (DIHB) and 8-(3-chlorophenyl)-2,6,7,8-tetrahydroimidazo[2,1-c][1,2,4]triazine-3,4-dione (HDIT) are promising candidates for anticancer agents, the first analytical procedures of which are presented in this paper. The commercially available unmodified glassy carbon electrode (GCE) was used as a sensor for the individual and simultaneous differential pulse voltammetric (DPV) determination of these possible anticancer drugs. The findings concerning the electrochemical behaviour indicated that DIHB and HDIT display at GCE, as a sensor, the oxidation peaks at 1.18 and 0.98 V, respectively (vs. Ag/AgCl, 3.0 mol L−1 KCl) in the 0.125 mol L−1 acetate buffer of pH = 4.5, which were employed for their quantification. Various experimental parameters were carefully investigated, to achieve high sensitivity in voltammetric measurements. Finally, under the optimised conditions (t of 60 s, ΔE A of 75 mV, ν of 225 mV s−1, and t m of 2 ms), the proposed DPV procedure with the GCE demonstrated broad linear sensing ranges (1–200 nmol L−1—DIHB and 5–200 nmol L−1—HDIT), boasting the detection limits of 0.18 nmol L−1 for DIHB and 1.1 nmol L−1 for HDIT. Moreover, the developed procedure was distinguished by good selectivity, repeatability of DIHB and HDIT signals and sensor reproducibility. The practical application of this method was demonstrated by analysing the urine reference material without any prior treatment. The results showed that this environmentally friendly approach, with a modification-free sensor, is suitable for the sensitive, selective and rapid quantification of DIHB and HDIT.

Ocimum basilicum is a valuable plant widely consumed worldwide and considered a rich source of polyphenols. This study examined the impact of the polyphenolic fraction isolated from basil (ObF) on human normal colon epithelial cells and human colorectal adenocarcinoma cells, evaluating its anti-inflammatory and protective activity against oxidative stress. The phytochemical characterization of the fraction was performed using ultra-performance liquid chromatography (UPLC) with a photodiode detector (DAD) and mass spectrometry (MS). UPLC-DAD-MS revealed that ObF predominantly contains caffeic acid derivatives, with rosmarinic acid and chicoric acid being the most abundant. The fraction demonstrated high antioxidant potential, as shown by DPPH assays, along with significant reducing power (FRAP). Furthermore, it prevented the depletion of antioxidant enzymes, including superoxide dismutase and catalase, and decreased malonylodialdehyde (MDA) in induced oxidative stress condition. Additionally, it exhibited a significant protective effect against H2O2-induced cytotoxicity in human normal colon epithelial cells. Although it had no impact on the viability of adenocarcinoma cells, it significantly reduced IL-1β levels in the neoplastic microenvironment. Our study demonstrated that basil polyphenols provide significant health benefits due to their antioxidant and protective activities.

In this work, a new voltammetric procedure for acyclovir (ACY) trace-level determination has been described. For this purpose, an electrochemically activated screen-printed carbon electrode (aSPCE) coupled with well-conductive electrolyte (CH3COONH4, CH3COOH and NH4Cl) was used for the first time. A commercially available SPCE sensor was electrochemically activated by conducting cyclic voltammetry (CV) scans in 0.1 mol L−1 NaOH solution and rinsed with deionized water before a series of measurements were taken. This treatment reduced the charge transfer resistance, increased the electrode active surface area and improved the kinetics of the electron transfer. The activation step and high conductivity of supporting electrolyte significantly improved the sensitivity of the procedure. The newly developed differential-pulse adsorptive stripping voltammetry (DPAdSV) procedure is characterized by having the lowest limit of detection among all voltammetric procedures currently described in the literature (0.12 nmol L−1), a wide linear range of the calibration curve (0.5–50.0 and 50.0–1000.0 nmol L−1) as well as extremely high sensitivity (90.24 nA nmol L−1) and was successfully applied in the determination of acyclovir in commercially available pharmaceuticals.

Carlina vulgaris is a poorly understood plant in the context of biological activity, despite its widespread application in ethnomedicine in numerous European countries. The aim of this study was to assess the cytotoxic potential of the plant against human colorectal adenocarcinoma (HT29) and to isolate the plant components linked to this effect. Ultra-high performance liquid chromatography with a high-resolution/quadrupole time-of-flight mass spectrometer (UHPLC–HR/QTOF/MS–PDA) was used for the phytochemical characterization of the extract. Liquid–liquid extraction and preparative chromatography were employed for fractionation purposes. Our investigation demonstrated that the ethyl acetate fraction from C. vulgaris showed significant cytotoxicity, and a bioactivity-guided approach led to the isolation of oxylipins, including traumatic acid, pinellic acid, and 9,10-dihydroxy-8-oxsooctadec-12-enic acid. The structures of the compounds were confirmed by nuclear magnetic resonance spectroscopy. Among these compounds, the last one exhibited significant cytotoxicity, though without selectivity, and traumatic acid was characterized by mild cytotoxicity. The cytotoxicity was linked to intracellular reactive oxygen species generation.

Carlina acaulis is highly valued in the traditional medicine of many European countries for its diuretic, cholagogue, anthelmintic, laxative, and emetic properties. Moreover, practitioners of natural medicine indicate that it has anti-cancer potential. However, its phytochemistry is still little known. In the present study, the polyphenolic composition of the plant was investigated using ultra-high-performance liquid chromatography coupled with a high-resolution/quadrupole time-of-flight mass spectrometer (UHPLC-HR/QTOF/MS-PDA). The fractionation of the extract was carried out using liquid-liquid extraction and preparative chromatography techniques. Cytotoxicity was assessed based on neutral red and MTT assays. The obtained data showed that the species is rich in chlorogenic acids and C-glycosides of luteolin and apigenin. The total amount of chlorogenic acids was 12.6 mg/g. Among flavonoids, kaempferol dihexosidipentose and schaftoside were the most abundant, reaching approximately 3 mg/g, followed by isoorientin, vitexin-2-O-rhamnoside, and vicenin II, each with a content of approximately 2 mg/g. Furthermore, the cytotoxic potential of the plant against human colorectal adenocarcinoma (HT29) and human cervical cancer (HeLa) cells was investigated using the normal epithelial colon cell line (CCD 841CoTr) as a reference. It has been demonstrated that the ethyl acetate fraction was the most abundant in polyphenolic compounds and had the most promising anticancer activity. Further fractionation allowed for the obtaining of some subfractions that differed in phytochemical composition. The subfractions containing polyphenolic acids and flavonoids were characterized by low cytotoxicity against cancer and normal cell lines. Meanwhile, the subfraction with fatty acids was active and decreased the viability of HeLa and HT29 with minimal negative effects on CCD 841CoTr. The effect was probably linked to traumatic acid, which was present in the fraction at a concentration of 147 mg/g of dried weight. The research demonstrated the significant potential of C. acaulis as a plant with promising attributes, thus justifying further exploration of its biological activity.

The paper presents a very simple way to extremely improve the sensitivity of trace V(V) determination. The application of a new supporting electrolyte composition (CH3COONH4, CH3COOH, and NH4Cl) instead of the commonly used acetate buffer (CH3COONa and CH3COOH) significantly enhanced the adsorptive stripping voltammetric signal of vanadium(V) at the lead-coated glassy carbon electrode (GCE/PbF). A higher enhancement was attained in the presence of cupferron as a complexing agent (approximately 10 times V(V) signal amplification) than in the case of chloranilic acid and bromate ions (approximately 0.5 times V(V) signal amplification). Therefore, the adsorptive stripping voltammetric system with the accumulation of V(V)–cupferron complexes at −1.1 V for 15 s in the buffer solution (CH3COONH4, CH3COOH, and NH4Cl) of pH = 5.6 ± 0.1 was selected for the development of a simple and extremely sensitive V(V) analysis procedure. Under optimized conditions, the sensitivity of the procedure was 6.30 µA/nmol L−1. The cathodic peak current of V(V) was directly proportional to its concentration in the ranges of 1.0 × 10−11 to 2.0 × 10−10 mol L−1 and 2.0 × 10−10 to 1.0 × 10−8 mol L−1. Among the electrochemical procedures, the lowest detection limit (2.8 × 10−12 mol L−1) of V(V) was obtained for the shortest accumulation time (15 s). The high accuracy of the procedure was confirmed on the basis of the analysis of certified reference material (estuarine water) and river water samples.

The dynamic production and usage of pharmaceuticals, mainly painkillers, indicates the growing problem of environmental contamination. Therefore, the monitoring of pharmaceutical concentrations in environmental samples, mostly aquatic, is necessary. This article focuses on applying screen-printed voltammetric sensors for the voltammetric determination of painkillers residues, including non-steroidal anti-inflammatory drugs, paracetamol, and tramadol in environmental water samples. The main advantages of these electrodes are simplicity, reliability, portability, small instrumental setups comprising the three electrodes, and modest cost. Moreover, the electroconductivity, catalytic activity, and surface area can be easily improved by modifying the electrode surface with carbon nanomaterials, polymer films, or electrochemical activation.

In this study, we present a simple, sensitive and selective analytical procedure for the ibuprofen (IBP) analysis using the commercially available screen-printed carbon electrode electrochemically activated (aSPCE) by cyclic voltammetry in 0.1 M NaOH. The quantitative determinations of IBP were carried out in 0.25 M acetate buffer solution of pH 4.5 ± 0.1 using the differential-pulse voltammetry (DPV). Different experimental parameters for DPV analysis were optimized, including pH and concentration of supporting electrolyte, amplitude (ΔEA), scan rate (ν) and modulation time (tm). The linear ranges of calibration curve were from 0.50–20.0 and 20.0–500.0 µM. The detection and quantification limits were estimated to be 0.059 and 0.20 µM. The aSPCE displayed satisfactory repeatability, reproducibility, and selectivity. Furthermore, the DPV procedure with the use of aSPCE was used to determination of IBP in pharmaceutical formulations. The results achieved by DPV show satisfactory agreement with those obtained by manufacturers (the relative errors are in the range of 3.1–4.7%).

Preparation of paraspinal tissue of patients with implants for elemental analysis is a challenge because it contains titanium in the ionic form, as well as metallic debris. Most literature reports focus on dissolving the tissue, but the impact of digestion conditions on metallic debris of Ti has not been investigated. In our work, various digestion conditions, including systems, compositions of oxidising mixture, and time, were tested aiming (i) to digest the tissue without digestion of metallic titanium to quantify soluble Ti and (ii) to digest metallic titanium debris to asses total Ti content in tissue. The experiments were performed in a closed mode using a microwave-assisted system and a carbon heating block. Our study revealed that total digestion of titanium was impossible in the tested conditions and the maximal level of digested titanium was below 70%. The mineralisation with the use of concentrated nitric acid was optimal to prepare paraspinal samples to analyse the soluble titanium form because metallic titanium passivated and did not migrate to the solution. The elaborated conditions were applied to determine titanium ion in the periimplant tissue of patients with three different titanium-based surgical systems, including traditional growing rod (TGR), guided growth systems (GGS), and vertical expandable prosthesis titanium rib (VEPTR).

A carbon nanofibers modified screen-printed carbon sensor (SPCE/CNFs) was applied for the determination of a novel promising anticancer agent candidate (ethyl 8-(4-methoxyphenyl)-4-oxo-4,6,7,8-tetrahydroimidazo[2,1-c][1,2,4]triazine-3-carboxylate, EIMTC) using square-wave voltammetry (SWV). It is the first method for the quantitative determination of EIMTC. The modified screen-printed sensor exhibited excellent electrochemical activity in reducing EIMTC. The peak current of EIMTC was found to be linear in two concentration ranges of 2.0 × 10−9 – 2.0 × 10−8 mol L−1 and 2.0 × 10−8 – 2.0 × 10−7 mol L−1, with a detection limit of 5.0 × 10−10 mol L−1. The connection of flow-cell for the SPCE/CNFs with SWV detection allowed for the successful determination of EIMTC in human serum samples. Ultra-high-performance liquid chromatography coupled to electrospray ionization triple quadrupole mass spectrometry (UHPLC-ESI-MS/MS) acted as a comparative method in the serum samples analysis.

Monolithic fillings used in chromatography are of great interest among scientists since the first reports of their synthesis and use were published. In the 20 years since silica-based monolithic columns were introduced into the commercial market, numerous papers describing their chromatographical properties and utility in various branches of industry and scientific investigations were presented. This review is focused on possible applications of commercially available silica-based HPLC monolithic columns in the analysis of biological samples.

Isoquinoline alkaloids are the main group of secondary metabolites present in Chelidonium majus extracts, and they are still the object of interest of many researchers. Therefore, the development of methods for the investigation and separation of the alkaloids is still an important task. In this work, the application potential of a silica-based monolithic column for the separation of alkaloids was assessed. The influence of the organic modifier, temperature, salt concentration, and pH of the eluent on basic chromatographic parameters such as retention, resolution between neighboring peaks, chromatographic plate numbers, and peak asymmetry were investigated. Based on the obtained results, a gradient elution program was developed and used to separate and quantitatively determine the main alkaloids in a Chelidonium majus root extract.

In this study, we compared the adsorption of methionine, cysteine and cystine at the mercury/chlorate (VII) interface. Changes in the surface tension with the potential of the zero charge γ z and relative surface excess Γ' of methionine, cysteine and cystine as a function of their concentration indicate that the adsorption of the studied amino acids increases in the order of methionine > cystine > cysteine. For all the systems examined, linear dependences ln[×(1–Θ)/Θ = f(Θ)] (Frumkin isotherm) and ln (Γ/c) = f(Γ') (virial isotherm) were obtained. Changes in the adsorption parameters as a function of the supporting electrolyte concentration indicate the competitive adsorption of amino acids and ClO 4 − ions and electrostatic interactions between the water dipoles and adsorbates in the double layer.

Ordered mesoporous carbon has been obtained by hard templating using SBA-15 and subsequently, oxidized (by treatment with ammonium persulphate) and thiol-functionalized (by treatment with thiol-contained polyhedral oligomeric silsesquioxane). Pristine and thiol-functionalized carbons were characterized by nitrogen adsorption, X-ray diffractometry, X-ray photoelectron spectroscopy, scanning electron microscopy and transmission electron microscopy and tested for their ability to adsorb bivalent heavy-metal ions (Cd, Cu, Pb, Zn) from the aqueous solutions. The observed static adsorption capacities are very high up to 0.76 mmol/g. Adsorption kinetics is also very fast: approximately 90% of the equilibrium amount is adsorbed after several minutes.