This study presents a novel and efficient high-performance liquid chromatography (HPLC) method for quantifying paracetamol in pharmaceutical products. The method utilizes a custom-fabricated monolithic column composed of poly(glycidyl methacrylate-co-ethylene glycol dimethacrylate-co-acrylic acid). The monolithic structure was synthesized in situ within a borosilicate glass capillary through ultraviolet (UV) polymerization at 365 nm. The resulting polymer matrix exhibited high porosity, which significantly enhanced surface area, permeability, and mass transfer efficiency-factors that contributed to improved chromatographic resolution and reduced analysis time. Chromatographic separation was achieved using a mobile phase consisting of acetonitrile and water (90:10, v/v) at a flow rate of 0.3 mL/min, with detection performed at a wavelength of 296 nm. The developed method demonstrated excellent linearity over a concentration range of 3 to 100 & micro;g/mL, with a correlation coefficient (R-2) of 0.9998. The calculated limits of detection (LOD) and quantification (LOQ) were 0.817 & micro;g/mL and 2.696 & micro;g/mL, respectively.
A novel series of Schiff bases, incorporating sulfonamide derivatives and 4-acyl-2-pyrazol-5-one, were synthesized using a simple condensation method. The structures of these newly synthesized compounds were comprehensively characterized through various techniques, including H-1 NMR, FT-IR, ESI-MS, elemental analysis and C-13 NMR spectroscopy. The structural properties of the studied molecules were investigated theoretically by carrying out Density Functional Theory (DFT). These newly synthesized compounds were then subjected to evaluation for their antibacterial activity against both gram +ve and gram-ve bacterial strains, as well as antioxidant assay. Additionally, they were screened for their in vitro anti-tubercular activity against Mycobacterium tuberculosis H37RV, with all results compared against a standard drug.
This study compared the phytochemical profiles and antioxidant activity of Platycladus orientalis when individually combined in a 1:1 ratio with Phyllanthus urinaria, Strobilanthes crispus, and Folium mori. The types of antioxidant interactions (synergistic, additive or antagonistic) in the combined plant samples were evaluated using both experimental and theoretical antioxidant capacity models. P. urinaria exhibited the highest phenolic content, reducing power, and radical scavenging potential, whereas S. crispus showed the lowest levels of phenolics, flavonoids, and antioxidant activity in the single-plant analysis. Pairing P. orientalis with the three selected medicinal plants resulted in either antagonistic or additive antioxidant effects, depending on the plant species and the sample concentration used. S. crispus contributed to the highest percentage of combined samples exhibiting an additive effect on total phenolic content, tannin levels, and reducing activity. The reducing activities of the combined plant samples were positively correlated with phenolic (r = 0.981) and flavonoid (r = 0.906) content, with high statistical significance (p < 0.0001). Pairing P. orientalis with either S. crispus or P. urinaria resulted in a relatively strong additive effect on reducing activity. Among the 108 combined plant samples, the mixture of P. orientalis (6.4 mg/mL) and S. crispus (6.4 mg/mL) exhibited the highest antioxidant index (97%) and an additive effect on overall phenolic content.
The increased demand for natural products within the agri-food sector has focused much research on the antifungal and antioxidant potentials of essential oils from aromatic plants. And by disrupting the cell membrane and fungi growth inhibition, these compounds have shown a great degree of antifungal activity on a wide variety of fungi and also stimulate plant immune systems. These substances have been reported to demonstrate activity against different pathogenic fungi. Essential oils such as those of Origanum vulgare, Thymus algeriensis, Eucalyptus globulus, and Rosmarinus officinalis with their major active principles such as thymol, carvacrol, eucalyptol, and eugenol represent the cluster of promising compounds due to their particular chemical composition. Additionally, they are high in antioxidants that protect cells from oxidative stress and help preserve food. Their application as natural antifungal agents presents several advantages, such as a broad spectrum of action, biodegradability and low toxicity for humans and the environment, which makes them a good candidate as food additives, in post-harvest treatment or in natural pesticide formulations.
Betulin is a significant triterpenoid known for its diverse and valuable pharmacological properties, including antiviral, antitumor, and antioxidant activities. The incorporation of a sulfate group enhances both the solubility and bioavailability of betulin. This study introduces a novel method for betulin sulfation utilizing a combination of ammonium sulfamate and urea. The resulting betulin sulfates were thoroughly analyzed through various techniques, including elemental analysis, infrared (IR) spectroscopy, X-ray diffraction, microscopy, and thermal analysis. The presence of the sulfate group was confirmed by FTIR spectroscopy, which revealed the emergence of specific absorption bands associated with sulfation. X-ray diffraction studies indicated a reduction in the crystallinity of the original betulin structure following sulfation. The findings from this research offer a fresh perspective on the sulfation process of betulin, suggesting its potential for enhanced application in pharmacology.
Phosphogypsum (PG) is an acidic by-product that is generated during the manufacture of phosphoric acid using the sulfuric acid route. The management of PG poses a significant environmental and human health challenge worldwide due to its huge quantity and chemical composition. This review offers an extensive analysis of the existing literature related to the wet conversion of gypsum, specifically PG, using potassium chloride (KCl), potassium carbonate (K2CO3), and potassium hydroxide (KOH) to produce potassium sulfate (K2SO4). Furthermore, we discuss the factors that influence these conversions, enabling a comparative study to identify the optimal conditions for achieving complete PG conversion. The economic feasibility and environmental implications of these three PG conversions are also examined and discussed.
Infectious disorders are among the dominant causes of death globally, and the beta-Lactams are the most effective antibiotics for managing these disorders. Unfortunately, Antimicrobial resistance has been frequently observed internationally, represented by the bacterial beta-lactamase which breaks down the beta-lactam ring, consequently disabling these drugs. The use of beta-lactamase inhibitors (e.g., clavulanic acid) combined with beta-lactams can minimize bacterial resistance. Therefore, these challenges necessitate the exploration for new remedies with potential antimicrobial and anti-beta-lactamase properties. This study utilizes docking design to synthesize and evaluate the antibacterial and anti-beta-lactamase activities of new non-beta-lactam 4,4'-methylenedianiline amides. The production of these amides was achieved through the reaction of carboxylic acids with 4,4'-methylenedianiline using the coupling agent N,N'-dicyclohexylcarbodiimide (DCC). After characterization of the new amides based on physical and spectral data, they were tested biologically against four strains of beta-lactamase-producing Gram-positive and Gram-negative bacteria to assess their anti-beta-lactamase activities and compared with that of clavulanic acid as a co-inhibitor with amoxicillin. The resulting data indicate that all the synthesized compounds exhibited varying degrees of activity against the beta-lactamases of all bacterial strains. The activity against P. aeruginosa was weaker than against Staph. aureus and E. coli. The observed activities were still weaker than that of the standard clavulanic acid. It has been determined that the beta-lactamase active site favors hydrophobic substituents, and halogen atoms and the nitro group enhance the binding of these hydrophobic residues and potentiate it.
Abstract: This study aims to identify the chemical constituents of Sinapis alba L. seeds essential oil and evaluate its antioxidant and anti-inflammatory activities. The chemicals were determined using Gas Chromatography-Mass Spectrometry (GC-MS), followed by predicting their biological potential in silico. Then, evaluation of their antioxidant activities in vitro using DPPH, FRAP, and Hydrogen Peroxide (H2O2) assays. Similarly, the anti-inflammatory activities were investigated through HRBC membrane stabilization, serum albumin denaturation, and proteinase inhibition assays. Our results showed that 3-butenyl isothiocyanate (58.36%), phenethyl isothiocyanate (0.95%), methallyl cyanide (0.64%), silane, ethenylethoxydimethyl- (0.51%), N-(3-methyl-2-butenyl)acetamide (0.50%), 4,5-epithiovaleronitrile (0.42%), and 3-carene (0.38%) were the major compounds revealed by GC-MS analysis. After passing the Lipinski rule, the compounds were predicted to be non-hepatotoxic agents, while the molecular docking manifested a great binding affinity between some target-ligand complex. Regarding the experimental study, S. alba essential oil showed significant antioxidant activity: DPPH (IC50 = 394.42 ± 0.01 mg/mL), H2O2 (IC50 = 498.81 ± 0.52 mg/mL), and FRAP (IC50 = 95.45 ± 0.03 mg/mL). Besides, the anti-inflammatory tests including HRBC membrane stabilization, serum albumin denaturation, and proteinase inhibition established values of 34.77 ± 0.08%, 95 ± 0.01%, and 50.61 ± 0.03%, respectively. Taken together, our results demonstrate that S. alba L. seeds essential oil have potential antioxidant as well as anti-inflammatory properties, that could be a scope for further research and potential use in pharmaceutical products.
Abstract: In our study, a unique "stability indicating high performance liquid chromatography" (HPLC) approach was developed for the measurement of elagolix, estradiol, and norethindrone concentrations in pharmaceutical capsule dosage forms. The separation was accomplished on a “Waters C18 column” (250 × 4.6 mm, 5 μm). The mobile phase including 0.1 M NaHSO4 (pH = 4.0) and pure methanol in a volume ratio of 60:40 v/v. The applied flow rate was 1.0 mL/min. The peaks detection and quantification on diode array detector were carried out at 248 nm wavelength. Capsule forms of elagolix, estradiol and norethindrone were exposed to hydrolytic (alkaline and acidic), oxidative, photo and thermal conditions. The retention times for elagolix, estradiol, and norethindrone were 3.206 min, 5.148 min, and 6.823 min, respectively. The proposed stability Indicating-HPLC-DAD approach was validated according to ICH guidelines and showed superior linearity with square of regression coefficient (R2) ˃ 0.999, reliable precision with relative standard deviation in the range of 0.091 to 0.709%, prominent accuracy between 99.130% and 101.323% recoveries and with lowly detection limit (0.008 µg/mL to 0.854 µg/mL) for all analytes. The specificity/stability indicative characteristics of HPLC-DAD approach were proved by peak homogeneity data in the stressed samples peaks acquired from the stressed capsule sample chromatograms. The validated stability Indicating-HPLC-DAD approach can be used for quality control and quality assurance of selected analytes in pharmaceutical oriahnn capsule dosage forms.
Abstract: The study conducted in Jericho and Al Aghwar Governorate, Palestine, aimed to assess the contents of Radium (226Ra) and Radon concentrations (222Rn) in 54 samples of drinking water taken from different locations. The closed can technique was employed for the measurements utilizing CR-39 Solid State Nuclear Track Detectors (SSNTDs) detectors. The average radon concentration ranges from 0.23 ± 0.02 to 2.26 ± 0.23 Bq/ℓ with a total average value of 0.88 ± 0.09 Bq/ℓ. The average value of radium contents varied from 11.1 ± 0.2 Bq/kg to 110.1 ± 1.5 Bq/kg with an overall mean value of 42.6 ± 0.6 Bq/kg. The recorded concentrations of 222Rn were found to be below the action levels established by both the US EPA and EU recommendations, which are set at 11 Bq/ℓ and 100 Bq/ℓ, respectively. However, it is important to note that these concentrations exceeded the maximum acceptable limit specified by the World Health Organization (WHO), which is documented as 0.4 Bq/ℓ. Consequently, the study concludes that consuming water from the investigated area, whether for drinking or cooking, is deemed safe and does not contain any significant health hazards. However, consuming water from the investigated area, whether for drinking or cooking, is considered safe and does not show any significant health risks for other types of water samples.
Abstract: Nauclea latifolia Sm. Rubiaceae is a native Southeast Nigerian tree known for its medicinal characteristics and is commonly found in various regions of Africa. N. latifolia is known to possess broad-spectrum medicinal bioactivities. In this assay the pulverized stem was extracted using methanol and chloroform. The extracts were analyzed using Gas Chromatography-Mass Spectrometry (GC-MS). The in vitro antimicrobial analysis was performed based on Broth dilution method using arrays of fungi and bacteria. A total of 10 and 12 compounds were isolated from the methanol and chloroform extracts, respectively, including docosanoic acid, arachidic acid, stearic acid, palmitic acid, oleic acid, and squalene. The methanolic extract showed activity against S. typhi with MBC/MIC ratio of 1.0 while the chloroform extract showed activity against S. mutans also with MBC/MIC ratio of 1.0. All other MBC/MIC ratios ranged from 2–8 while those of the fungi was from 1.0 to 4.0 for both extracts. Our results were comparable to those of the standard drugs. Therefore, N. latifolia stem extracts contained phytochemicals of relevance in ethnomedicine.
This research work presents a comprehensive analysis to examine the dynamic changes in the nutritional profile, antioxidant capability, and heavy metal accumulation of tomatoes during the ripening process. Tomatoes (Solanum lycopersicum L.) are a widely consumed fruit, making it a priority to ensure their nutritional composition and safety. Advanced statistical methods were employed to examine the factors inducing the ripening process. The research study reveals how these factors change, providing insights into the nutritional quality and safety of tomatoes. The results show a consistent increase in several parameters from stage S1 to S4 of ripening: titratable acidity (0.205-0.385%), moisture content (93.24-95.79%), total sugar content (TSC) (546.44-631.84 mg/100 g) and total carotenoids (93.12-134.75 ppm). Additionally, total flavonoid content (TFC) (715.34-906.86 mg/100 g), total phenolic content (TPC) (943.34-1172.54 mg/100 g) and antioxidant activity measured through RPA (1710.58-1775.28 mg/100 g) and DPPH radical scavenging assay (19.32-78.80% inhibition) assessment, also increase from S1 to S4. The analysis of heavy metals shows higher accumulation of zinc (Zn) and iron (Fe) in both tomatoes and soil samples, but levels remain below permissible limits, indicating food safety. The study highlights significant correlations between the nutritional profile, antioxidant capacity, and heavy metal accumulation, as well as presenting insights into the parameters affecting tomatoes' nutritional value and quality. Moreover, the research investigates the impact of ripening on heavy metal accumulation, crucial for ensuring food safety. The consideration of these dynamics informs strategies to minimize health risks from heavy metal exposure through diet. Generally, this comprehensive analysis enhances knowledge of the nutritional dynamics and safety of ripening tomatoes, contributing to better agricultural practices, food processing and dietary recommendations, ultimately promoting public health and food security.
One of the illnesses afflicting some people worldwide is sickle cell disease which transcends national and ethnic boundaries. In this study, similar compounds from phenanthrene-9,10-dione were obtained using the SwissSimilarity prediction model with fingerprint and pharmacophore as the screening methods. Nine similar compounds were obtained with a similarity score ranging from 1.0 to 0.75. These compounds were subjected to SwissADME and optimized with DFT. Four out of the nine compounds failed ADMET studies. The remaining five compounds with good DFT and ADMET properties were subjected to molecular docking and molecular dynamic simulations. 3-phenylphenanthrene-9,10-dion 3-phenylphenanthrene-9,10-dione (A9-4) had the best binding affinities with the three proteins; A9-4 had-11.0 kcal/mol,-10.9 kcal/mol, and-8.0 kcal/mol, compared to Rivaroxanban binding affinities of-8.5 kcal/mol,-8.1 kcal/mol, and-8.0 kcal/mol with crystal structure and binding pocket of Carbonmonoxy Sickle Hemoglobin in R-State Conformation, crystal structure and binding pocket of carboxyhemoglobin and crystal structure and binding pocket of destabilize sickle hemoglobin polymer formation (PDB IDs 5E6E, 6BWU, and 6D14), respectively. Molecular dynamic simulations showed that the complex formed between the protein and 3-phenylphenanthrene-9,10-dione (A9-4) is more stable than the complex formed with Rivaroxanban.
This groundbreaking study investigates the presence of organochlorine pesticide (OCP) residues by using GC-EI/MS, in the most widely consumed natural fruit and vegetable juices from Jordanian local markets and assesses the related health risks for both children and adults. A total of 50 samples were collected in 2023 from ten different types of juices. Nine pesticide residues, including alpha-HCH, (3-HCH, gamma-HCH, aldrin, Endosulfan-I, dieldrin, endrin, P,P '-DDD and P,P '-DDE, were detected at varying concentrations. These ranged from 0.03 mu g/L for aldrin in lemon juice to 8.11 mu g/L for (3-HCH in orange juice. Most residues were found to be within the maximum residue limits (MRLs) set by regulatory authorities. The total burden of OCPs in the juices ranked as follows: orange (2.30 mu g/L) > pineapple (2.14 mu g/L). A comprehensive evaluation of the total cancer risk (CR), health quotient (HQ) and hazard index (HI) was conducted for both children and adults. The findings revealed that the hazard index (HI) for orange and tomato juice samples exceeded unity for children, indicating potential health risks. Specifically, the CR for orange juice ranged from 1.04 x 10(-)(3) to 6.26 x 10(-)(5), while for tomato juice, it ranged from 3.39 x 10(-)(4) to 1.46 x 10(-)(5) in children. These values suggest that orange and tomato juices contained the highest levels of OCP contamination among the studied samples. Consequently, these juices could pose significant chronic health risks, particularly for children, who may consume larger quantities relative to their body weight. The study underscores the importance of monitoring pesticide residues in fruit and vegetable juices to mitigate potential health risks, especially for vulnerable populations like children, who may be more susceptible to the adverse effects of prolonged exposure to OCPs in Jordan.
Deep eutectic solvents are widely used in various science related fields including organic chemistry, electrochemistry and etc. In this work, we present results regarding preparation of new deep eutectic solvents-a mixture of ammonium sulfamate (ASA) with urea (U) and its derivatives (methyl urea (MetU), ethyl urea (EtU), hydroxyethyl urea (HEtU). Melting points of various components eutectic mixtures are determined and phase diagrams are presented. It is shown that the eutectic point temperature of the ammonium sulfamate with urea (urea mole fraction 0.3) mixture is 361 degrees K, with methyl urea mixture is 358 degrees K (mole fraction 0.7), with ethyl urea mixture-362 degrees K (mole fraction 0.6), with the hydroxyethyl urea-354 degrees K (mole fraction 0.6). Based on obtained experimental data a complex calculation of the thermodynamic characteristics of the system (enthalpy, entropy, chemical potential, effective interaction parameter) was carried out. The chemical potentials of a deep eutectic solvent were calculated using ideal and real solution models.
The genus Oxalis is known for its diverse medicinal properties, offering phytochemicals with therapeutic applications. This study investigates the potential of these compounds as modulators of human pregnane X receptor (hPXR), a key regulator of genes involved in drug metabolism and detoxification. Its activation affects the body's response to foreign chemicals (xenobiotics), including drugs, influencing drug-drug interactions, pharmacokinetics, and toxicity. Using molecular docking techniques, 36 compounds selected from Oxalis corniculata and Oxalis latifolia were evaluated for their interaction with hPXR. The phytocomponents, squalene, diosmetin-7-O-beta-D-glucopyranoside, apigenin-7-O-glucoside, rhapontin, and luteolin-7-O-glucoside exhibited stronger binding affinities compared to the receptor's native ligand, suggesting a better role in modulating hPXR activity. Protein-ligand interaction analysis of five ligands revealed hydrophobic, hydrogen bonds, and salt bridges, with key residues, TRP299, HIS407, LEU209, LEU411 and PHE288, stabilizing ligand binding. ADMET analysis predicted favorable drug-like properties for these compounds, supporting their further development. Squalene, diosmetin-7-O-beta-D-glucopyranoside, and apigenin-7-O-glucoside were identified as promising candidates due to their strong binding and acceptable pharmacokinetic profiles. This computational evaluation provides insights into Oxalis phytochemicals as potential natural modulators of hPXR, with implications for therapeutic interventions and future experimental studies.
This study delves into the refractive index of binary mixtures of (Bmim.Triflate) with 1-butanol and 1-pentanol, which is key to unlocking deeper insights into the molecular interactions that drive innovations in chemical synthesis, catalysis, and energy storage. Using high-precision experimental measurements, we ensured accurate refractive index data across varying mole fractions and temperatures. Traditional mixing rules, such as Arago-Biot and Lorentz-Lorenz, were tested for refractive index prediction but showed limitations in accuracy. To overcome these challenges, we harnessed the power of machine learning (ML), employing a polynomial regression model to accurately capture the nonlinear relationships among the mole fraction, temperature, and refractive index. The ML models significantly outperform conventional methods, delivering highly precise predictions with low mean absolute errors (MAEs) and high R2 values for both 1-butanol and 1-pentanol. This study highlights the transformative potential of machine learning in predicting complex physical properties, offering a flexible and more accurate approach to optimizing processes in cutting-edge applications.
Disinfecting drinking water is crucial for protecting human health. The objective of this study is to monitor disinfection BrO(3)(-)by-product and Br-, which result from the reaction of ozone used as a disinfectant in certain drinking water sources, including ozonized bottled, well, and tap water. The ion chromatography high-performance liquid chromatography (IC-HPLC) was used to quantify BrO(3)(-)and Br(- )in different drinking water samples (well, tap, and ozonated bottled water) collected in Erbil city Kurdistan Region of Iraq. In this investigation, the Br-concentrations in ozonated, well, and tap water were between 12.3 to 31245 mu g L-1. The results of this study indicated that most samples had Br(- )levels below the detection limit. However, 25% of the analyzed samples had BrO(3)(- )concentrations ranging from 11 to 33.1 mu g L-1, exceeding the maximum allowable limit set by the WHO and EPA (10 mu g L-1). As a result, individuals consuming these ozonated bottled water are at an increased risk of cancer.
In present work, a simple, accurate and precise RP-HPLC method was developed and validated for simultaneous estimation of Sofosbuvir and Velpatasvir in tablets. A systematic Quality by Design (QbD) approach was employed to optimize the chromatographic parameters, using rotatable central composite design for multivariate analysis. The method's critical parameters, including acetonitrile percentage, flow rate and column temperature were optimized to achieve acceptable resolution and system suitability with enhanced accuracy and precision. The quadratic models obtained for each response, enabling a detailed understanding of the factors influencing method performance. The ANOVA confirmed the significance of the models and the adequacy of the equations, with flow rate and organic phase concentration being the most critical factors affecting retention time and resolution. The method was validated in accordance with ICH guidelines, demonstrating good linearity, accuracy, precision, sensitivity and specificity of sofosbuvir and velptasvir. The method's robustness, combined with its validated accuracy and precision, makes it suitable for routine quality control analysis in pharmaceutical formulations.
Chemical substances referred to as nitrosamines have the potential to negatively impact DNA, induce cancer, as well as damage the liver and kidney. It is vitally necessary to analyze these chemical components in pharmacological substances. The investigation of synthetic process of rivaroxaban revealed the likely production of four nitrosamine impurities (NDSRI-Imp-1 to NDSRI-Imp-4) related to rivaroxaban synthesis. This work came up with a sensitive and feasible LC-MS/MS approach for determining NDSRI-Imp-1 to NDSRI-Imp-4 simultaneously in rivaroxaban. For separation and analysis, the YMC Pack triart PFP (250 mm x 4.6 mm, 3 mu m) column, and aqueous (0.1%) formic acid (aqueous phase solvent) and acetonitrile (organic phase solvent) as solvent phases of mobile phase in gradient elution mode were used. The proposed LC-MS/MS methodology was also validated in line with ICH Q2 (R2) criteria. The LC-MS/MS approach was effectively executed on three rivaroxaban batch samples. The linearity was found between 0.0091 to 0.0609 ppm (NDSRI-Imp-1), 0.0088 to 0.0584 ppm (NDSRI-Imp-2), 0.0080 to 0.0534 ppm (NDSRI-Imp-3), and 0.0091 to 0.0606 ppm (NDSRI-Imp-4). For all nitrosamine impurities under study, the limits of quantification were determined between 0.0080-0.0091 ppm, respectively. The range of nitrosamine recoveries in the rivaroxaban sample was 85.4-96.8%, with a precision of 1.26% to 9.62% RSD. The impurities NDSRI-Imp-1 to NDSRI-Imp-4 were verified using infrared, proton and carbon nuclear magnetic resonance and mass spectrometry. The carcinogenic potency grouping (category 4) of impurities NDSRI-Imp-1 to NDSRI-Imp-4 was done. The technique (LC-MS/MS) described here may be extremely helpful in determining the NDSRI-Imp-1 to NDSRI-Imp-4 present in RRXN. The assessment of impurities NDSRI-Imp-1 to NDSRI-Imp-4 rivaroxaban batch samples indicated that the impurities NDSRI-Imp-1 to NDSRI-Imp-4 are below detectable limits.
