Search Results (22)

Extracts from natural waste like bark or leaves are great sources of phytochemicals, which contain functional groups (hydroxyl, carboxylic, vinyl, allyl) attractive in terms of polymer synthesis. In this study, the synthesis of epoxy with an extract of Scots pine bark as a natural co-hardener was evaluated. Ultraviolet-visible (UV-Vis) spectroscopy was used for the identification of phytochemicals with conjugated dienes and quantification of TPC. Also, the total solid content (TSC) of representative extracts was calculated. The best extract in terms of total phenolic content (TPC) value was selected as a co-hardener and investigated using differential scanning calorimetry (DSC) for thermal effects and attenuated total reflectance Fourier transform infrared spectroscopy (ATR FTIR) for reactions between functional groups. Also, the mechanical properties (flexural modulus, flexural strength, impact strength, Shore D hardness) and density of composition were obtained for extract-based epoxy and compared to reference sample values. Results were discussed in terms of future research and improvement of compositions. Also, potential applications were proposed. Full article

Graphene oxide (GO) has shown significant potential in humidity sensing. It is well accepted that the oxygen-containing functional groups in GO significantly influence its humidity sensing performance. However, the relationship between the content of these groups and the humidity sensing capability of GO-based sensors remains unclear. In the present work, we investigate the role of oxygen-containing functional groups in the humidity sensing performance by oxidizing graphite with mesh numbers 80–120, 325, and 8000 using the Hummers method, resulting in GO-80, GO-325, and GO-8000. Infrared spectroscopy (IR) and X-ray photoelectron spectroscopy (XPS) were used to identify the types and quantification of oxygen-containing functional groups. Molecular dynamics simulation is used to simulate the adsorption energy, intercalation dynamics, and hydrogen bonding of water molecules. Electrochemical tests were used to compare the adsorption/desorption time and response sensitivity of graphene oxide to humidity. It is proposed that hydroxyl and carboxyl groups are the main contributing groups to humidity sensing. GO-8000 shows a relatively fast response time, but the large number of carboxyl groups will hinder intercalation of water molecules, thus exhibiting lower sensitivity. This research provides a reference for the future development of graphene-based sensors, catalysts, and environmental materials. Full article

Pyrethroid pesticides (PYRs) have found widespread application in agriculture for the protection of fruit and vegetable crops. Nonetheless, excessive usage or improper application may allow the residues to exceed the safe limits and pose a threat to consumer safety. Thus, there is an urgent need to develop efficient technologies for the elimination or trace detection of PYRs from vegetables. Here, a simple and efficient magnetic solid-phase extraction (MSPE) strategy was developed for the simultaneous purification and enrichment of five PYRs in vegetables, employing the magnetic covalent organic framework nanomaterial COF-SiO₂@Fe₃O₄ as an adsorbent. COF-SiO₂@Fe₃O₄ was prepared by a straightforward solvothermal method, using Fe₃O₄ as a magnetic core and benzidine and 3,3,5,5-tetraaldehyde biphenyl as the two building units. COF-SiO₂@Fe₃O₄ could effectively capture the targeted PYRs by virtue of its abundant π-electron system and hydroxyl groups. The impact of various experimental parameters on the extraction efficiency was investigated to optimize the MSPE conditions, including the adsorbent amount, extraction time, elution solvent type and elution time. Subsequently, method validation was conducted under the optimal conditions in conjunction with gas chromatography–mass spectrometry (GC-MS). Within the range of 5.00–100 μg·kg⁻¹ (1.00–100 μg·kg⁻¹ for bifenthrin and 2.5–100 μg·kg⁻¹ for fenpropathrin), the five PYRs exhibited a strong linear relationship, with determination coefficients ranging from 0.9990 to 0.9997. The limits of detection (LODs) were 0.3–1.5 μg·kg⁻¹, and the limits of quantification (LOQs) were 0.9–4.5 μg·kg⁻¹. The recoveries were 80.2–116.7% with relative standard deviations (RSDs) below 7.0%. Finally, COF-SiO₂@Fe₃O₄, NH₂-SiO₂@Fe₃O₄ and Fe₃O₄ were compared as MSPE adsorbents for PYRs. The results indicated that COF-SiO₂@Fe₃O₄ was an efficient and rapid selective adsorbent for PYRs. This method holds promise for the determination of PYRs in real samples. Full article

Sorbitol derivatives and other additives are commonly used in various products, such as packaging or food packaging, to improve their mechanical, physical, and optical properties. To accurately and precisely evaluate the efficacy of adding sorbitol-type nucleating agents to these articles, their quantitative determination is essential. This study systematically investigated the quantification of sorbitol-type nucleating agents in food packaging made from impact copolymers of polypropylene (PP) and polyethylene (PE) using attenuated total reflectance infrared spectroscopy (ATR-FTIR) together with analysis of principal components (PCA) and machine learning algorithms. The absorption spectra revealed characteristic bands corresponding to the C–O–C bond and hydroxyl groups attached to the cyclohexane ring of the molecular structure of sorbitol, providing crucial information for identifying and quantifying sorbitol derivatives. PCA analysis showed that with the selected FTIR spectrum range and only the first two components, 99.5% of the variance could be explained. The resulting score plot showed a clear pattern distinguishing different concentrations of the nucleating agent, affirming the predictability of concentrations based on an impact copolymer. The study then employed machine learning algorithms (NN, SVR) to establish prediction models, evaluating their quality using metrics such as RMSE, R², and RMSECV. Hyperparameter optimization was performed, and SVR showed superior performance, achieving near-perfect predictions (R² = 0.9999) with an RMSE of 0.100 for both calibration and prediction. The chosen SVR model features two hidden layers with 15 neurons each and uses the Adam algorithm, balanced precision, and computational efficiency. The innovative ATR-FTIR coupled SVR model presented a novel and rapid approach to accurately quantify sorbitol-type nucleating agents in polymer production processes for polymer research and in the analysis of nucleating agent derivatives. The analytical performance of this method surpassed traditional methods (PCR, NN). Full article

Pb endangers forest ecological health; phytoremediation is an effective Pb remediation technology. Woody plants with Pb tolerance provided a mechanism for the phytoremediation of Pb. Paulownia fortunei (L.), a fast-growing woody plant, has a good tolerance to Pb. However, its tolerance mechanism is unclear. The results in this study revealed that P. fortunei seedlings can withstand 400 mg·L⁻¹ Pb stress. The quantification of Pb in different P. fortunei tissues showed an increasing trend of accumulation in root > leaf > stem; the transport coefficient and enrichment coefficient decreased with an increase in Pb concentration. The tolerance of P. fortunei to Pb may be related to cell partition and immobilization by the cell wall. Microstructural analysis performed using scanning electron microscopy showed that the absorbed Pb is mainly distributed in cell wall components, and when the concentration of Pb increases, it can be transferred to soluble parts and organelles. The Fourier transform infrared spectrometry results showed that excess hydroxyl groups occurred under Pb stress in the outer epidermis cell walls of roots and leaves adsorbing heavy metals. When the concentration of Pb was over 400 mg·L⁻¹, the growth of P. fortunei was inhibited, the root cell wall was deformed, the plasmolysis occurred in the cauline cell, and the internal leaf capsule was ruptured. Furthermore, antioxidant enzyme activity was significantly reduced. Therefore, P. fortunei can transfer the underground part of Pb to the aboveground part up to the concentration of 400 mg·L⁻¹. This study provides a theoretical basis and technical reference for fully utilizing woody plant resources to restore the ecological environment of forests. Full article

In this work, a conductive hydrogel was successfully synthesized, taking advantage of the high number density of active amino and hydroxyl groups in carboxymethyl chitosan and sodium carboxymethyl cellulose. These biopolymers were effectively coupled via hydrogen bonding with the nitrogen atoms of the heterocyclic rings of conductive polypyrrole. The inclusion of another biobased polymer, sodium lignosulfonate (LS), was effective to achieve highly efficient adsorption and in-situ reduction of silver ions, leading to silver nanoparticles that were embedded in the hydrogel network and used to further improve the electro-catalytic efficiency of the system. Doping of the system in the pre-gelled state led to hydrogels that could be easily attached to the electrodes. The as-prepared silver nanoparticle-embedded conductive hydrogel electrode exhibited excellent electro-catalytic activity towards hydroquinone (HQ) present in a buffer solution. At the optimum conditions, the oxidation current density peak of HQ was linear over the 0.1–100 μM concentration range, with a detection limit as low as 0.12 μM (signal-to-noise of 3). The relative standard deviation of the anodic peak current intensity was 1.37% for eight different electrodes. After one week of storage in a 0.1 M Tris-HCl buffer solution at 4 °C, the anodic peak current intensity was 93.4% of the initial current intensity. In addition, this sensor showed no interference activity, while the addition of 30 μM CC, RS, or 1 mM of different inorganic ions does not have a significant impact on the test results, enabling HQ quantification in actual water samples. Full article

A study of keracyanin chloride (KC) electrochemical behavior in an aqueous buffer solution using screen-printed carbon electrodes (SPCEs) and glassy carbon electrodes (GCEs) was performed. Cyclic voltammetry (CV) and square-wave voltammetry (SWV) were used to analyze the electrochemical response of KC under studied conditions. A clear redox wave was observed for KC, primarily due to the oxidation of the catechol 3′,4′-dihydroxyl group of its ring B, with a minor redox wave from oxidation of the hydroxyl groups in ring A. Compared to GCEs, using modified SPCEs resulted in two-fold amplification in the electrochemical oxidation signal of KC. Using SPCEs as a working electrode could provide high sensitivity in the quantification of KC and the ability to gauge KC quantification to significantly lower detection limits. Full article

Stera-3β,5α,6β-triols make useful tracers of the autoxidation of Δ⁵-sterols. These compounds are generally analyzed using gas chromatography–mass spectrometry (GC-MS) after silylation. Unfortunately, the 5α hydroxyl groups of these compounds, which are not derivatized by conventional silylation reagents, substantially alter the chromatographic properties of these derivatives, thus ruling out firm quantification of trace amounts. In this work, we developed a derivatization method (trifluoroacetylation) that enables derivatization of the three hydroxyl groups of 3β,5α,6β-steratriols. The derivatives thus formed present several advantages over silyl ethers: (i) better stability, (ii) shorter retention times, (iii) better chromatographic properties and (iv) mass spectra featuring specific ions or transitions that enable very low limits of detection in selected ion monitoring (SIM) and multiple reaction monitoring (MRM) modes. This method, validated with cholesta-3β,5α,6β-triol, was applied to several environmental samples (desert dusts, marine sediments and particulate matter) and was able to quantify trace amounts of 3β,5α,6β-steratriols corresponding to several sterols: not only classical monounsaturated sterols (e.g., cholesterol, campesterol and sitosterol) but also, and for the first time, di-unsaturated sterols (e.g., stigmasterol, dehydrocholesterol and brassicasterol). Full article

Hydroxylated polychlorinated biphenyls (OH-PCBs) are a group of metabolites biotransformed from polychlorinated biphenyls by animals with higher toxicities than their parent compounds. The present work developed and validated an analytical method for determinating penta-, hexa-, and hepta-chlorine substituted OH-PCBs in animal-derived food based on ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) with isotope-dilution. The target analytes were extracted with a 50% n-hexane/dichloromethane (v/v), purified by sulfuric acid-silica gel, and separated by 5% hydrated silica gel, achieving a final concentration of 100 times before injection to LC–MS/MS. The limits of detection (LOD) and quantification (LOQ) for target OH-PCBs were within the ranges of 0.003–0.010 μg/kg and 0.009–0.030 μg/kg, respectively. Average recoveries ranged between 76.7% and 116.5%, with relative standard deviations of less than 18.4%. The proposed method is simple, time-saving, sensitive, and accurate, making it a powerful tool for risk monitoring of OH-PCBs in animal-derived food. Full article

Neurotransmitters (NTs) with hydroxyl groups can now be identified electrochemically, utilizing a variety of electrodes and voltammetric techniques. In particular, in monoamine, the position of the hydroxyl groups might alter the sensing properties of a certain neurotransmitter. Numerous research studies using electrodes modified on their surfaces to better detect specific neurotransmitters when other interfering factors are present are reviewed to improve the precision of these measures. An investigation of the monoamine neurotransmitters at nanoscale using electrochemical methods is the primary goal of this review article. It will be used to determine which sort of electrode is ideal for this purpose. The use of carbon materials, such as graphite carbon fiber, carbon fiber micro-electrodes, glassy carbon, and 3D printed electrodes are only some of the electrodes with surface modifications that can be utilized for this purpose. Electrochemical methods for real-time detection and quantification of monoamine neurotransmitters in real samples at the nanomolar level are summarized in this paper. Full article

The chemical exchange saturation transfer (CEST) signal at −1.6 ppm is attributed to the choline methyl on phosphatidylcholines and results from the relayed nuclear Overhauser effect (rNOE), that is, rNOE(−1.6). The formation of rNOE(−1.6) involving the cholesterol hydroxyl is shown in liposome models. We aimed to confirm the correlation between cholesterol content and rNOE(−1.6) in cell cultures, tissues, and animals. C57BL/6 mice (N = 9) bearing the C6 glioma tumor were imaged in a 7 T MRI scanner, and their rNOE(−1.6) images were cross-validated through cholesterol staining with filipin. Cholesterol quantification was obtained using an 18.8-T NMR spectrometer from the lipid extracts of the brain tissues from another group of mice (N = 3). The cholesterol content in the cultured cells was manipulated using methyl-β-cyclodextrin and a complex of cholesterol and methyl-β-cyclodextrin. The rNOE(−1.6) of the cell homogenates and their cholesterol levels were measured using a 9.4-T NMR spectrometer. The rNOE(−1.6) signal is hypointense in the C6 tumors of mice, which matches the filipin staining results, suggesting that their tumor region is cholesterol deficient. The tissue extracts also indicate less cholesterol and phosphatidylcholine contents in tumors than in normal brain tissues. The amplitude of rNOE(−1.6) is positively correlated with the cholesterol concentration in the cholesterol-manipulated cell cultures. Our results indicate that the cholesterol dependence of rNOE(−1.6) occurs in cell cultures and solid tumors of C6 glioma. Furthermore, when the concentration of phosphatidylcholine is carefully considered, rNOE(−1.6) can be developed as a cholesterol-weighted imaging technique. Full article

The search for new ways to obtain analogues of the well-known Methylene Blue dye is an important synthetic task. Herein, we proposed and developed an approach to the synthesis of 3-N′-arylaminophenothiazines and asymmetrical 3,7-di(N′-arylamino)phenothiazines. This approach included the optimization of synthetic strategy by quantification analysis of the positive charge distribution in the cation of 3-N′-arylaminophenothiazine derivative. The obtained experimental data are confirmed by DFT studies. Two synthetic routes for asymmetrical phenothiazine diarylamino derivatives were suggested and verified. The developed convenient and versatile synthetic approach makes it easy to obtain aromatic Methylene Blue isostructural analogues with various substituents. As a result, a series of novel 3-N′-arylaminophenothiazines and asymmetrical 3,7-di(N′-arylamino)phenothiazines containing ester, tert-butoxycarbonyl, sulfonic acid, hydroxyl and amine groups were obtained in high yields. Full article

8-Hydroxypyrene-1,3,6-trisulfonate (HPTS) is a small, hydrophilic fluorescent molecule. Since the pKa of the hydroxyl group is close to neutrality and quickly responds to pH changes, it is widely used as a pH-reporter in cell biology for measurements of intracellular pH. HPTS fluorescence (both excitation and emission spectra) at variable pH was measured in pure water in the presence of NaCl solution or in the presence of different buffers (PBS or hepes in the presence or not of NaCl) and in a solution containing BSA. pKa values have been obtained from the sigmoidal curves. Herein, we investigated the effect of mono-, di-, and trivalent cations (Na⁺, Ca²⁺, La³⁺, Gd³⁺) on fluorescence changes and proposed its use for the quantification of trivalent cations (e.g., gadolinium ions) present in solution as acqua-ions. Starting from the linear regression, the LoD value of 6.32 µM for the Gd³⁺ detection was calculated. The effects on the emission were also analyzed in the presence of a combination of Gd³⁺ at two different concentrations and the previously indicated mono and di-valent ions. The study demonstrated the feasibility of a qualitative method to investigate the intracellular Gd³⁺ release upon the administration of Gd-based contrast agents in murine macrophages. Full article

Hesperidin (HESP) is a plant bioflavonoid found in various nutritional and medicinal products. Many of its multiple health benefits rely on the compound’s antioxidant ability, which is due to the presence of oxidizable hydroxyl groups in its structure. Therefore, the present study aimed to investigate the electrochemical behavior of HESP at a cheap, disposable pencil graphite electrode (PGE) in order to develop rapid and simple voltammetric methods for its quantification. Cyclic voltammetric investigations emphasized a complex electrochemical behavior of HESP. The influence of the electrode material, solution stability, supporting electrolyte pH, and nature were examined. HESP main irreversible, diffusion-controlled oxidation signal obtained at H type PGE in Britton Robinson buffer pH 1.81 was exploited for the development of a differential pulse voltammetry (DPV) quantitative analysis method. The quasi-reversible, adsorption-controlled reduction peak was used for HESP quantification by differential pulse adsorptive stripping voltammetry (DPAdSV). The linear ranges of DPV and DPAdSV were 1.00 × 10⁻⁷–1.20 × 10⁻⁵ and 5.00 × 10⁻⁸–1.00 × 10⁻⁶ mol/L with detection limits of 8.58 × 10⁻⁸ and 1.90 × 10⁻⁸ mol/L HESP, respectively. The DPV method was applied for the assessment of dietary supplements bioflavonoid content, expressed as mg HESP. Full article

Diosmin (DIO) is a naturally occurring flavonoid with multiple beneficial effects on human health. The presence of different hydroxyl groups in diosmin structure enables its electrochemical investigation and quantification. This work presents, for the first time, diosmin voltammetric behavior and quantification on the cost-effective, disposable pencil graphite electrode (PGE). Diosmin oxidation on PGE involves two irreversible steps, generating products with reversible redox behaviors. All electrode processes are pH-dependent and predominantly adsorption-controlled. Differential pulse (DPV) and adsorptive stripping differential pulse (AdSDPV) voltammetric methods have been optimized for diosmin quantification o an H-type PGE, in 0.100 mol/L H₂SO₄. The linear ranges and limits of detection were for DPV 1.00 × 10⁻⁶–1.00 × 10⁻⁵ mol/L and 2.76 × 10⁻⁷ mol/L DIO for DPV and 1.00 × 10⁻⁷–2.50 × 10⁻⁶ mol/L and 7.42 × 10⁻⁸ mol/L DIO for AdSDPV, respectively. The DPV method was successfully applied for diosmin quantification in dietary supplement tablets. The percentage recovery was 99.87 ± 4.88%. Full article