Attenuated Total Reflectance Fourier Transform Infrared Spectroscopy Research Articles

Diimide-Mediated Hydrogenation of Nitrile Butadiene Rubber

The hydrogenation of nitrile butadiene rubber (NBR) has shown great potential for improving its physical, thermal, mechanical, and chemical stability. Hydrogenation process of NBR in this work involved the utilization of diimide produced from the interaction between hydrazine hydrate (N2H4) and hydrogen peroxide (H2O2), with the addition of boric acid as a promoter. Attenuated total reflectance Fourier transform infrared (ATR-FTIR), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), and X-ray diffraction (XRD) were used to evaluate the degree of hydrogenation, glass transition, thermal stability, and rubber crystallinity, respectively. The highest hydrogenation degree was 99%, which resulted in a 57% gel content. Upon hydrogenation, both the glass transition temperature (Tg) and decomposition temperature (Td) increased. The hydrogenated rubber samples generally showed an amorphous state, except for the 99% hydrogenated sample, which displayed a semi-crystalline state. However, using diimide for direct hydrogenation yields a side reaction from the free radicals in the system, which leads to gel formation. Optimization was accomplished by employing the response surface methodology (RSM), which entailed manipulating parameters such as the total solid content (TSC) of NBR, reaction time, and the mole ratio of H2O2 to N2H4, to reduce the percentage of gel content. The RSM analysis identified the optimum reaction conditions as a 1:1 mole ratio of H2O2: N2H4 and 25% TSC, with a reaction time of 8 h, which yielded 32% gel content percentage, where a mole ratio of H2O2 to N2H4 and reaction time indicated a synergistic effect, whereas TSC denoted an antagonistic effect.

Investigation of new analysis methods for simultaneous and rapid identification of five different microplastics using ATR-FTIR spectroscopy and chemometrics

Microplastic (MP) pollution in water has become one of the most important global problems of our time. The development of appropriate and rapid analysis techniques is of great importance at the beginning of the studies aimed at solving this problem. In the presented study, in order to perform the qualitative and quantitative analysis of MP forms of polyamide (PA), polyethylene (PE), polypropylene (PP), polystyrene (PS), and polyethylene terephthalate (PET), which are known to be most abundant in water, in a fast and easy way, new Attenuated Total Reflectance-Fourier Transform Infrared (ATR-FTIR) spectroscopy methods were tried to be developed by utilizing chemometric methods. While principal component analysis (PCA) was applied for qualitative analyses, partial least squares (PLS) models were created for quantitative analyses. Raw, 1st, and 2nd order derivatives of all spectra and their spectra with different levels of smoothing points were taken and 24 different chemometric models were created for each MP. In interpreting the statistical performances of the developed PCA and PLS models, different parameters were used. According to the obtained results, the qualitative discrimination of all polymer types was successfully achieved. It was determined that the PLS models developed for the quantitative determination of mixtures consisting of different concentrations of MP types could not be at the desired level. However, it was determined that the PLS models developed for PA, PE, PP, and PET, where the normal spectrum was used, could give quantitatively accurate results, albeit partially.

Antimicrobial gelatin-based films with cinnamaldehyde and ZnO nanoparticles for sustainable food packaging

Cinnamaldehyde (CIN), a harmless bioactive chemical, is used in bio-based packaging films for its antibacterial and antioxidant properties. However, high amounts can change food flavor and odor. Thus, ZnO nanoparticles (NPs) as a supplementary antimicrobial agent are added to gelatin film with CIN. The CIN/ZnO interactions are the main topic of this investigation. FTIR-Attenuated Total Reflection (ATR), X-ray diffraction (XRD), and scanning electron microscopy (SEM) were utilized to investigate CIN/ZnO@gelatin films. Transmission electron microscope (TEM) images revealed nanospheres morphology of ZnO NPs, with particle sizes ranging from 12 to 22 nm. ZnO NPs integration increased the overall activation energy of CIN/ZnO@gelatin by 11.94%. The incorporation of ZnO NPs into the CIN@gelatin film significantly reduced water vapour permeability (WVP) of the CIN/ZnO@gelatin film by 12.07% and the oxygen permeability (OP) by 86.86%. The water sorption isotherms of CIN/ZnO@gelatin were described using Guggenheim-Anderson-de Boer (GAB) model. The incorporation of ZnO NPs into the CIN@gelatin film reduced monolayer moisture content (M0) by 35.79% and significantly decreased the solubility of CIN/ZnO@gelatin by 15.15%. The inclusion of ZnO into CIN@gelatin film significantly decreased tensile strength of CIN/ZnO@gelatin by 13.32% and Young`s modulus by 18.33% and enhanced elongation at break by 11.27%. The incorporation of ZnO NPs into the CIN@gelatin film caused a significant decrease of antioxidant activity of CIN/ZnO@gelatin film by 9.09%. The most susceptible organisms to the CIN/ZnO@gelatin film included Candida albicans, Helicobacter pylori, and Micrococcus leutus. The inhibition zone produced by the CIN/ZnO@gelatin film versus Micrococcus leutus was 25.0 mm, which was comparable to the inhibition zone created by antibacterial gentamicin (23.33 mm) and cell viability assessment revealed that ZnO/CIN@gelatin (96.8 ± 0.1%) showed great performance as potent biocompatible active packaging material.

Determination of spectroscopy marker of atherosclerotic carotid stenosis using FTIR-ATR combined with machine learning and chemometrics analyses

Atherosclerotic carotid stenosis (ACS) is a recognized risk factor for ischemic stroke. Currently, the gold diagnostic standard is Doppler ultrasound, the results of which do not provide certainty whether a given person should be qualified for surgery or not, because in some patients, carotid artery stenosis, for example at the level of 70 %, does not cause ischemic stroke in others yes. Therefore, there is a need for new methods that will clearly indicate the marker qualifying the patient for surgery. In this article we used Fourier Transform InfraRed Attenuated Total Reflectance (FTIR-ATR) spectra of serum collected from healthy and patients suffering from ACS, which had surgery were analyzed by machine learning and Principal Component Analysis (PCA) to determine chemical differences and spectroscopy marker of ACS. PCA demonstrated clearly differentiation between serum collected from healthy and non-healthy patients. Obtained results showed that in serum collected from ACS patients, higher absorbances of PO2− stretching symmetric, CH2 and CH3 symmetric and asymmetric and amide I vibrations were noticed than in control group. Moreover, lack of peak at 1106 cm−1 was observed in spectrum of serum from non-control group. As a result of spectral shifts analysis was found that the most important role in distinguishing between healthy and unhealthy patients is played by FTIR ranges caused by vibrations of PO2− phospholipids, amides III, II and CO lipid vibrations. Continuing, peaks at 1636 cm−1 and 2963 cm−1 were proposed as a potential spectroscopy markers of ACS. Finally, accuracy of obtained results higher than 90 % suggested, that FTIR-ATR can be used as an additional diagnostic tool in ACS qualifying for surgery.

Analysis and discrimination of adhesive species using ATR-FTIR combined with Raman, and HS-GC-IMS together with multivariate statistical analysis

Identifying the species and origin of adhesives in criminal investigations aids in narrowing inquiry scope and supporting case detection. This study introduces two advanced combined analytical techniques for distinguishing adhesive species, including attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR) combined with Raman spectroscopy, and headspace gas chromatography-ion mobility spectrometry (HS-GC-IMS) together with multivariate statistical analysis. ATR-FTIR categorized seven adhesives into three groups based on the base materials, with further differentiation achieved via Raman spectra. Analysis of volatile components identified 79 volatile organic compounds (VOCs), with esters being the most concentrated. The fingerprint profile clearly illustrated the characteristic fingerprint sequence and unique marker compounds of each adhesive, effectively enabling their differentiation. Multivariate statistical analysis methods, including principal component analysis (PCA), orthogonal partial least squares discriminant analysis (OPLS-DA), heatmap, and hierarchical cluster analysis (HCA), were utilized to visually interpret the classification of adhesives. This integrated analytical approach provides a comprehensive analysis of adhesive compositions, facilitating the diversification and precision of adhesive species identification, and broadening the scope for detecting and analyzing trace evidence in forensic science.

Microplastic detectives: a citizen-science project reveals large variation in meso- and microplastic pollution along German coastlines

Plastic production and plastic waste have increased to such an extent that it has become globally ubiquitous. Several studies already have investigated the meso- and microplastic pollution along the German Baltic and North Sea coasts, but were all limited to a few locations. To obtain representative bulk samples from sandy beaches along the entire German coast, we initiated a citizen-science project entitled “Microplastic Detectives.” Here, we describe in detail 1) how we recruited, instructed, and engaged citizen scientists, 2) why we chose bulk sampling over reduced-volume sampling, and 3) the laboratory methods we used. The citizen scientists collected 1,139 samples from 71 locations along the German coast, totalling 2.2 tons of sand. After drying, sieving with a 1 mm sieve, and visual inspection of the retained fraction under a binocular microscope, all putative plastic particles ≥1 mm were analysed by attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectroscopy. 177 out of 1,139 samples (15.5%) contained a total of 260 plastic particles, with a large right-skewed variation among locations. Most of the particles were fragments, foils, foams, fibres, and pellets (96.2% in total), and 89.6% of the particles were made of polyethylene, polypropylene, polyester, and polystyrene. The unweighted mean pollution densities were 4.12 particles m−2, 0.17 particles kg−1 and 0.27 particles L−1, and the weighted mean pollution densities were 3.77 particles m−2, 0.11 particles kg−1 and 0.18 particles L−1. These densities are lower than in other similar studies, but previous studies had important methodological differences. We discuss how these differences could have influenced the results and make recommendations for improving future studies. Two important recommendations are 1) to use random or stratified random sampling and 2) to run transects perpendicular (rather than parallel) to the waterline. Our study highlights that large-scale, scientifically rigorous monitoring of meso- and microplastic pollution is possible at the national level, and possibly even at much larger spatial and temporal scales. With the help of local authorities, such a monitoring program could be established.

Authentication of a Painting Attributed to the Rembrandt School

This paper presents the archaeometric and chemometric authentication of a Renaissance-style oil painting on linen canvas, with plaster and barium sulphate-based primer preparation and bone glue as binder. By optical microscopy (OM), stereomicroscopy (SOM), scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM-EDX) and attenuated total reflectance–Fourier transform infrared spectroscopy (ATR-FTIR), a series of archaeometric characteristics were identified: the grain size of the chemical components of the paint layers, the 3D porosity distribution of the pigments, the degree of penetration between the paint layers and the varnish and between the varnish and the oxidatively anchored dirt, and the typology of the craquelure (craquelure network arrangement and morphology). By correlating the results obtained, it was possible to estimate the period of the painting as 1660 ± 3 years.

Preparation of Mesoporous Analcime/Sodalite Composite from Natural Jordanian Kaolin

In this work, a meso-macroporous analcime/sodalite zeolite composite was produced by a hybrid synthesis process between a complex template method and hydrothermal treatment at 220 °C of naturally abundant kaolinitic-rich clay, using dodecyltrimethylammonium bromide as an organic soft template to enhance the mesoporous structure. The chemical and morphological properties of the developed zeolites composite were characterized using powder X-ray diffraction (PXRD), attenuated total Reflectance–Fourier transform infrared spectroscopy (ATR-FTIR), thermogravimetric analysis (TGA), N2 adsorption/desorption; and scanning electron microscopy with energy dispersive spectroscopy (SEM-EDS) methods were used to study the morphology, chemical composition and structure of the product. Two types of zeolite particles were obtained:(1) hollow microsphere with an attached analcime icositetrahedron of 30–40 µm in size and (2) sodalite microsphere with a ball-like morphology of 3–4 µm in size. Both N2 adsorption/desorption and surface area data confirmed the high potentiality of the produced zeolite composite to act as an excellent adsorbent to remove inorganic pollutants such as Cu, Cd, Cr, Ni, Zn, and Pb ions, organic pollutants such as dyes, phenolic compounds, and surfactants from water; and their high catalytic activity, especially in the oxidation reaction of volatile organic compounds. The catalytic activity and adsorption ability of the produced analcime/sodalite composite will be tested experimentally in future work.

Attenuated Total Reflection-Fourier Transform Infrared (ATR-FTIR) Spectroscopy Analysis of Saliva as a Diagnostic Specimen for Rapid Classification of Oral Squamous Cell Carcinoma Using Chemometrics Methods

Background & Aim Recent advancements in analytical techniques have highlighted the potential of Attenuated Total Reflection-Fourier Transform Infrared (ATR-FTIR) spectroscopy as a quick, cost-effective, non-invasive, and efficient tool for cancer diagnosis. This study aims to evaluate the effectiveness of ATR-FTIR spectroscopy in combination with supervised machine learning classification models for diagnosing OSCC using saliva samples. Methods & Materials Eighty unstimulated whole saliva samples from OSCC patients and healthy controls were collected. The ATR-FTIR spectroscopy was performed and spectral data were used to classify healthy and OSCC groups. The data were analyzed using machine learning classification methods such as Partial Least Squares-Discriminant Analysis (PLS-DA) and Support Vector Machine Classification (SVM-C). The classification performance of the models was evaluated by computing sensitivity, specificity, precision, and accuracy. Results The samples were classified into two classes based on their spectral data. The obtained results demonstrate a high level of accuracy in the prediction sets of the PLS-DA and SVM-C models, with accuracy values of 0.960 and 0.962, respectively. The OSCC group sensitivity values for both PLS-DA and SVM-C models was 1.00, respectively. Conclusion The study indicates that ATR-FTIR spectroscopy, combined with chemometrics, is a potential method for the non-invasive diagnosis of OSCC using saliva samples. This method achieved high accuracy and the findings of this study suggest that ATR-FTIR spectroscopy could be further developed for clinical applications in OSCC diagnosis.

CHANGES IN SECONDARY STRUCTURE OF PROTEIN IN SKELETAL MUSCLE DUE TO HIGH-CARBOHYDRATE OR HIGH-FAT DIETS

Objective: Obesity, which arises from changes in lifestyle and feeding habits, is a threat to human health. One essential contributor to the increase in obesity rates is the popularity of high-calorie diets. This study aims to investigate high-fat (HFD) and high-carbohydrate (HCD) diet-induced molecular changes in protein secondary structure in longissimus dorsi skeletal muscle tissues of female inbred C57BL/6J mice by utilizing Attenuated Total Reflectance-Fourier Transform Infrared (ATR-FTIR) spectroscopy. Materials and Methods: Mice were fed a control diet, HCD, or HFD for 24 weeks. Their skeletal muscle tissues were collected, and their spectra were recorded using a Bruker Invenio S ATR-FTIR spectrometer in the 4000-400 cm-1 region. Results: The protein secondary structure profiles of the HCD group demonstrated a significant rise in antiparallel β-sheet and β-turn and a decline in parallel β-sheets together with the insignificant increase in aggregated β-sheets and a decrease in α-helix. The impact of an HFD on protein conformation is less pronounced than HCD. The HFD diet led to an increase in antiparallel β-sheets and a decrease in parallel β-sheets. Although it was not significant, an increase was observed in β-turn and α-helix. Conclusion: These results propose the appearance of protein aggregation and/or formation of protein-protein intermolecular interaction in skeletal muscle tissues of female inbred C57BL/6J mice. Collectively, these data suggest that both high-calorie diets impair secondary structures of protein in skeletal muscle that may affect its metabolic function.

Modulation of charge structure in Bi/Bi2O3-In2O3@C for efficient CO2 electroreduction to formate

Electrocatalytic CO2 reduction reaction (ECO2RR) to value-added chemicals is of significant importance to control CO2 emission and reach carbon neutrality. Herein, Bi/Bi2O3-In2O3@C electrocatalyst with nanosheet arrays is successfully fabricated by a facile solvothermal with subsequent calcination process. It is found that the electron structure of Bi/Bi2O3-In2O3@C can be adjusted by the synergistic effects of Bi-In hetero-diatoms, which can significantly enhance its inherent catalytic activity. As expected, it requires a maximum HCOOH faradaic efficiency (FEHCOOH) of 97.6 % at −1.1 V vs. Reversible Hydrogen Electrode (RHE), which further delivers over 90 % at a wide potential range of −0.8 to −1.4 V vs. RHE, and exhibits high stability of 90.1 % over 60-h long-term test. In-situ Raman analysis is performed to explore the mechanism of its excellent stability. Meanwhile, in-situ attenuated total reflection-Fourier-transform infrared (ATR-FTIR) analysis combined with theoretical calculations reveal that the hetero-bridging absorption of *OCHO and d-d orbital coupling effect can regulate d-band center of Bi/Bi2O3-In2O3@C and improve its density of states around Ef, moderating free energy of intermediates, thereby the improved formate production performance can be seen.

Biopolyurethane coatings with silica-titania microspheres (MICROSCAFS®) as functional filler for corrosion protection

In this work, we studied a biopolyurethane (BioPU) coating derived from a bio-based polyol and isocyanate for the protection of carbon steel against corrosion. The direct utilization of polyols obtained from raw biomass represents a novelty in polyurethane coatings production. The protective properties of these coatings were enhanced by incorporating unique silica-titania (ST) MICROSCAFS®, which are microspheres exhibiting interconnected macro- and mesoporosity. They were loaded with tannic acid (TA), an eco-friendly corrosion inhibitor. Confirmation of TA loading into the ST carriers (therefore called ST\\TA) was achieved through Attenuated total reflectance - Fourier-transform infrared spectroscopy (ATR-FTIR) and Thermogravimetric (TG) analyses. TG analysis revealed that ST\\TA particles contain approximately 34 wt% TA, and their average particle diameter is approximately 25 ± 5 μm, observed by SEM. The TGA shows slightly improved thermal resistance of the coatings modified with the filler MICROSCAFS®. Furthermore, it was observed that the fillers strengthened the coating hardness without negatively affecting the adhesion strength. Electrochemical Impedance Spectroscopy (EIS) results demonstrated that all modified coatings exhibited very good to excellent resistance in mild corrosive environments. The coatings maintained a high impedance modulus (|Z|) at low frequencies and phase angle values close to −90° across a wide frequency range, over an immersion period of 80 days in a 0.05 M NaCl solution. After 80 days of immersion, the best coating, BPU-ST\\TA, displayed |Z| of 3 × 1010 Ω cm2. Scanning Vibrating Electrode Technique (SVET) analysis revealed the inhibitory behaviour of TA. For the BPU-ST\\TA sample, inhibition of both anodic and cathodic activities was clearly visible, with a significant reduction of the current densities starting at 1 h and up to at least 24 h of immersion. In summary, the BioPU coatings modified with tannic acid-loaded MICROSCAFS® exhibit improved barrier properties and notable corrosion inhibition capacity in mild corrosive environments.

Microplastic-contamination in the flesh and gastrointestinal tract of nile tilapia (Oreochromis niloticus) reared in floating net cages at lake Ranu Grati, Pasuruan, East Java, Indonesia

In recent years, microplastics (MPs) have emerged as a prominent environmental problem in waters and environments, including lake waters. Microplastics in freshwater, such as those in floating net cages (FNC), can be consumed by Nile tilapia (Oreochromis niloticus), one of the commercially available cultivated fish in Indonesia. This study aims to determine the prevalence of microplastics and compare their characteristics in the surface water, flesh, and gastrointestinal tract (GIT) of Nile Tilapia (O. niloticus) at Lake Ranu Grati, Pasuruan, East Java, Indonesia. Visual characteristics of MPs were observed using a stereo microscope, and polymers were analysed by ATR-FTIR (Attenuated Total Reflection-Fourier Transform Infrared Spectroscopy). The abundance of MPs from water sample locations in Lake Ranu Grati reached 1116 MPs particles. In the water samples, the inner and outer sides of the FNC are dominated by the MPs with a size range of 251–500 µm and 1001-2000 µm in the milieu of Ranu Grati Lake. The most common MPs' types and colours are fibre and black, dominated by Polyethylene (PE). In 25 O. niloticus samples, 576 particles of MPs were found in the flesh and 724 particles in the gastrointestinal tract (GIT). This study found no significant variation in microplastic abundance between flesh and GIT samples (p>0.05; Mann-Whitney U test). Microplastics in Nile Tilapia flesh samples were dominated by blue fibres with a size range of 101–250 µm, and the polymer found was PA (polyamide). Meanwhile, in the GIT samples, microplastics were dominated by black fibre, with a size range of 251–500 µm, and the polymer found was PA (polyamide).

The Application of Wood Biowaste Chemically Modified by Bi2O3 as a Sorbent Material for Wastewater Treatment

Textile dyes discharged into aquatic systems can have significant environmental impacts, causing water pollution and toxicity to aquatic life, and constituting a human health risk. To manage these effects, the sorption ability of wood biowaste chemically modified by Bi2O3 for textile dye removal was investigated. Sorbent characterization was performed using scanning electron microscopy, and elemental analysis by energy dispersive X-ray spectroscopy (SEM-EDX), X-ray diffraction (XRD), the Brunauer–Emmett–Teller (BET) method for the specific surface area, and Fourier transform infrared spectroscopy–attenuated total reflectance (FTIR-ATR). The optimization of the sorption process was carried out, and optimal parameters, such as contact time, pH, the dose of sorbent, the concentration of dye, and temperature, were defined. Also, desorption studies were conducted. Kinetics and isotherms studies were carried out, and the data fits to a pseudo-second order model (r2 ≥ 0.99) and Langmuir model (r2 ≥ 0.99), indicating that the process occurs in the monolayer form and the dye sorption depends on the active sites of the sorbent surface. The maximal sorption capacity of the sorbent was 434.75 mg/g.

Quantitative Analysis of the Li-Ion Solvation Structure in Li-Ion Battery Electrolytes Using ATR-FTIR Spectroscopy.

Attenuated total reflection-Fourier transform infrared (ATR-FTIR) spectroscopy is widely used to study condensed materials due to its convenient sample preparation and ability to avoid absorption saturation. Recently, it has been applied to in situ and in operando observations of chemical reactions within electrochemical devices, such as lithium-ion batteries. However, because ATR-FTIR spectroscopy relies on frequency-dependent attenuated reflectance, quantitative concentration measurements of chemical species using the Beer-Lambert law are challenging. Despite the availability of several correction methods, discrepancies remain in the solvation structures around Li+ ions when comparing transmission-type FTIR and ATR-FTIR spectroscopy results, which complicate the determination of solvation and desolvation energies. In this study, we investigate ATR-FTIR correction algorithms, elucidate the reasons for the discrepancies between ATR-FTIR and transmission FTIR spectroscopy results, and develop a method to correct the ATR-FTIR spectrum to accurately determine the solvation structures around Li+ ions.

Amine-functionalized cellulose-silica composites for the remediation of hexavalent chromium (Cr IV) in contaminated water

Adsorption method for Hexavalent chromium (Cr(VI) removal from domestic and industrial wastewater is widely desirable due to public health concern of the heavy metal. The purpose of this study was to investigate the evaluation of Cr(VI) adsorption using a novel adsorbent: amine-functionalized cellulose-silica composite derived from banana fibers. We employed the in-situ sol–gel method to create cellulose-silica silane functionalized composites, analyzing them through different characterization techniques such as Attenuated total reflectance- Fourier transform infrared spectroscopy (ATR-FTIR), X-ray Diffraction Analysis (XRD), Thermo gravimetric analysis (TGA)/differential thermogravimetric (DTG), Brunauer–Emmett–Teller (BET), Scanning Electron Microscopy (SEM), and Transmission Electron Microscopy (TEM) techniques. ATR-FTIR depicted key organic constituents in raw banana pseudo stem fibers (BF) and the formation of SiO bonds in BCSiO2 composite, and further enhanced by the grafting of N-[3-(trimethoxysilyl)propyl ethylenediamine (DAPTMS) onto the BC-SiO2 surface in BC-SiO2-DAPTMS. XRD and TGA/DTG analyses revealed changes in crystallinity and thermal stability, while BET analysis showcased altered surface area and pore characteristics in BC-SiO2-DAPTMS (2 %). SEM and TEM imaging provided visual evidence of structural modifications and improved dispersion in BC-SiO2-DAPTMS composites. The impact of composite weight, contact time, and pH on Cr(VI) removal rates was examined, revealing optimal performance at slightly acidic pH 4 value (80.7 %) and enhanced efficiency with increased contact time of 65 min (86.66 %), composite weight of 1 g (82.62 %), and initial concentration was for 0.8 mg/l (80 %). The kinetics and isotherms analyzed using pseudo second order (PSO) and pseudo first order (PFO) models, highlight the composite’s efficiency. The Freundlich model was found to better fit the adsorption isotherm data, while the PSO model described the kinetics more accurately. These insights contribute to optimizing the BC-SiO2-DAPTMS (2 %) composite for efficient Cr(VI) ion removal in water treatment applications.

Development, Validation, and Greenness Assessment of HPLC and ATR-FTIR for Mangiferin Quantitative Analysis in Raw Material

Due to the benefits of mangiferin, including antidiabetic, antibacterial, antiviral, antioxidant, and anti-inflammatory activities, it is a natural raw material used in botanical health and cosmetic products. This research aims to develop and validate analytical methods for the quantification of mangiferin in raw material, isolated from Mangifera indica L. leaves, using high performance liquid chromatography (HPLC) and attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR). The greenness assessment of both analytical methods was performed. The results indicated that both methods were validated in terms of specificity, linearity, range, detection limit, quantitation limit, accuracy, and precision. The ranges of mangiferin used in HPLC and ATR-FTIR were 30 to 360 µg/mL and 5.00 to 27.27% w/w, respectively. The mangiferin content in five batches, analyzed by using the validated HPLC and ATR-FTIR, ranged from 88.35 to 109.4% w/w and 90.7 to 111.8% w/w, respectively. Statistical analysis using a paired t-test revealed no significant difference in the mangiferin quantity between the two techniques at a 95% confidence level. The greenness scores of the HPLC and ATR-FTIR determined according to AGREE metric were 0.49 and 0.81, respectively. Both methods can be applied to quantify mangiferin content and control the quality of mangiferin raw material. Additionally, the validated ATR-FTIR, which proposed excellent environmental friendliness, was suggested as an alternative analytical method for routine assay of mangiferin raw material.

PolyPyrrole based-impedimetric aptasensor for selective determination of beta-HCG from urine sample

Herein, a conjugated conducting polymer-based impedimetric aptasensor has been developed to detect beta-human chorionic gonadotropin (bHCG), the one of the important biomarkers in gynecology, from synthetic human urine samples. In this context, gold electrodes were, firstly coated with pyrrole and pyrrole-3-carboxylic acid to obtain the poly(pyrrole-pyrrole-3-carboxylic acid) [poly(Py-PyCOOH)] conductive copolymer by cyclic voltammetry (CV). Then, bHCG-specific peptide aptamer was covalently linked onto the surface via applying a well-known carbodiimide-succinimide chemistry. The sensor developed was characterized to confirm modification steps via both electrochemical methods including CV, electrochemical impedance spectroscopy (EIS), and chronoamperometry and physico-chemically via attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDX), atomic force microscope (AFM), and contact angle measurements (CA). The analytical performance of the sensor was evaluated in the concentration range from 1 μg/mL to 100 μg/mL for successful detection of bHCG even in the presence of interference agents. The results have also revealed that the sensor could be classified as a promising alternative to its benchmark commercial clinical methods due its superior properties such as cost-friendliness, easy-to-prepare, stable, robust, and selectivity / sensitivity.

Green formulation of Menadione-loaded niosome as a skin-lightening preparation: In vitro/In vivo safety evaluation on Wistar rat

Purpose: In the present research, a green technique (an ultrasonic method) was used to synthesize menadione sodium bisulfite (MSB) niosome (Menasome) which is used to improve dermal delivery and increase anti-melanogenesis activities. Methods: Various cholesterol: surfactant (Chol: Sur) ratios were investigated to optimize the Menasomes. Photon correlation spectroscopy, attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR), transmission electron microscopy (TEM), and differential scanning calorimetry (DSC) were employed to characterize the solid state of MSB in nanoparticle form. Additionally, the optimized formulation was used to investigate ex-vivo skin absorption, in vivo skin irritation, in vitro cell survival, and anti-melanogenesis activity. Results: The results exhibited that increasing cholesterol (Chol) declined the average size of the Menasomes from 653.766±25.171 nm to 298.133±8.823 nm and increased entrapment efficiency 30.237±3.4204% to 83.616±2.550 %. The rat skin permeation study indicated that Menasome gel administered more MSB in dermal layers (439.000±36.190μg/cm2 or 23.827±1.964%) than MSB plain gel (286.200± 22.6μg/cm2 or 15.53±1.227%). In both the in vivo skin irritation test and the in vitro cytotoxicity experiment, the extended-release behavior of the enhanced Menasome demonstrated a minimal side effect profile. Furthermore, optimum Menasome inhibited melanin formation (37.426± 1.644% at 15μM) greater than free MSB (57.383±1.654%) considerably (p <0.05). Furthermore, Menasome 7 prevented L-dopa auto-oxidation in higher levels (95.140±2.439%) than pure MSB solution (83.953±1.629%). Conclusion: According to the study's findings, the prepared Menasome could be employed as a viable nanovehicle for MSB dermal delivery, a promising solution for the management of human hyperpigmentation disorders.

Determination of antioxidant capacity and phenolic content of haskap berries (Lonicera caerulea L.) by attenuated total reflectance-Fourier transformed-infrared spectroscopy

The total phenolic content (TPC) and antioxidant capacity (TAC) of haskap berries cultivated in various locations across Alberta were analyzed using attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectroscopy. The Folin–Ciocalteu assay was used to determine TPC, while TAC was quantified by 2,2-diphenyl-1-picrylhydrazl radicals (DPPH) assay and oxygen radical absorbance capacity (ORAC) assay. Three tenfold cross-validated partial least-squares regression (PLSR) models and three fivefold cross-validated deep learning models were developed separately based on FT-IR spectra collected from 22 haskap berry samples and their corresponding reference values determined through Folin-Ciocalteu, DPPH, and ORAC assays. The deep learning models (R2 = 0.95, 0.93, and 0.90 for Folin-Ciocalteu, DPPH, and ORAC assays, respectively) demonstrated better prediction capability compared to the PLSR models (R2 = 0.74, 0.72, and 0.66 for Folin-Ciocalteu, DPPH, and ORAC assays, respectively). In addition, PLS loading plots indicated that phenolic contents and polysaccharides in haskap berries could contribute to their antioxidant capacity. Using ATR-FTIR to estimate the TPC and TAC of fruits offers a rapid alternative to the conventional chemical assays.