Objective: Nifurtimox is a type of nitrofuran derivative employed for treating sleeping sickness as well as Chagas disease. The aim is to develop and validate a precise and specific liquid chromatography mass spectrometric technique for the estimation of Nifurtimox in human plasma.Material and Method: Chromatographic separation had been accomplished on reverse-phase C18 (4.6 mm × 100 mm, 3.5 µm) column employing benznidazole as an internal standard along mobile phase made up of methanol and 5 mM aqueous ammonium acetate in a 75:25 (v/v) ratio at a flow rate of 0.8 ml/min in isocratic mode. A quadrupole mass spectrometer running in positive mode and with numerous reaction monitoring settings was employed to quantify the procedure.Result and Discussion: The developed analytical method exhibited good recovery and was validated over a calibration range of 0.5–400 ng/ml. In the ESI spectra, the major ion peaks for Nifurtimox and the internal standard, benznidazole, were observed at m/z 288 and m/z 261, respectively, corresponding to their [M+H]+ ions. The method exhibited LOD, LOQ, and LLOQ of 0.2 ng/ml, 1.0 ng/mL and 0.5 ng/ml respectively. Precision at intra and interday and accuracy were evaluated at low (1 ng/ml), medium (50 ng/ml), and high (400 ng/ml) quality control levels, showing a %RSD below 2. The percentage recoveries exceeded 95%, with %RSD values under 2. Overall, the validated method is suitable for routine quantification of Nifurtimox in biological samples.

The primary aim of the current investigation was the Analytical progression and validation of a UV-spectrophotometric analytical approach for the quantification of Nirogacestat in both bulk and pharmaceutical dosage forms, in alignment with ICH regulatory standards. A straightforward, expeditious, reliable, and economically viable UV-spectrophotometric technique was established for the quantitative determination of Nirogacestat employing acetonitrile as the solvent medium. The absorbance of the analyte solution was recorded at 269 nm relative to a suitable blank. Method validation was performed pursuant with prescribed parameters, encompassing linearity, accuracy, precision and robustness. The λmax of Nirogacestat in acetonitrile was identified at 269 nm. The analyte demonstrated compliance with Beer-Lambert’s law across the concentration interval of 2.5–15.0 μg/mL, exhibiting a correlation coefficient(R²) of 0.999. The percentage recovery ranged from 99.3% to 100.1% reflecting substantial accuracy. Precision assessments resulted %RSD values below 2.0, substantiating both repeatability and intermediate precision. Robustness evaluations involving minor alterations in wavelength exhibited negligible deviation, thereby affirming reliability. Additionally, forced degradation experiments substantiated the stability-indicating characteristics. The delineated UV-spectrophotometric technique is straightforward, analytically sensitive, and reproducible. It is eminently suitable for routine quality assessment and quantitative evaluation of Nirogacestat in bulk drug substances and tablet formulations.

Enmetazobactam and cefepime were determined quantitatively in bulk materials and pharmaceutical formulation using a quick, simple, accurate, QbD HPLC Greenness approach. Greenness measurement evaluates how environmentally benign an analytical method is across its life cycle by applying Green Analytical Chemistry (GAC) principles to quantify impacts from solvents/reagents (toxicity and amounts), waste generation, energy use, sample throughput, miniaturization, and automation. Separation was accomplished by using Box-Behnken design by varying column temperature, flow rate and ratio of propylene carbonate. Chromatographic separation was done using a Waters X-Bridge Phenyl column (250 × 4.6 mm, 5 μm) utilized upon an e2695 system from Waters Alliance. 0.1

The present study explores the phytochemical and biological potential of Hymenocallis littoralis, combining computational and laboratory investigations. Phytochemical analysis confirmed the presence of alkaloids, glycosides, tannins, flavonoids, steroids, and phenolic compounds as key bioactive constituents. SWISSADMET predictions revealed that all twelve selected compounds exhibit favorable pharmacokinetic properties, adhering to Lipinski’s Rule of Five and demonstrating high gastrointestinal solubility. Network pharmacology analyses using KEGG Pathway and Cytoscape identified HSP90AA1, HIF1A, and HSP90AB1 as highly interacting proteins with the selected compounds, with HIF1A recognized as a critical inflammation-related target. Molecular docking studies highlighted Quercetin 5,7,3',4'-tetramethyl ether 3-rutinoside (-10.3 kcal/mol) and Hippeastrine (-9.9 kcal/mol) as potent inhibitors of the inflammatory target protein 4BQG. In vitro evaluations demonstrated significant anti-inflammatory activity of the ethyl acetate fraction of Hymenocallis littoralis. These findings collectively indicate that Hymenocallis littoralis, particularly its ethyl acetate fraction, holds substantial therapeutic potential for inflammation management and related disorders

A robust and repeatable RP-HPLC technique has been created for the concurrent measurement of Bupivacaine as well as Meloxicam in pharmaceutical formulation. The method underwent validation following applicable regulatory guidelines. The optimized chromatographic conditions included the use of a C18 Zorbax SB column (250x4.6 mm, 5 µ), an isocratic mobile phase comprising acetonitrile and a hexane sulfonic acid (2.5 pH adjusted with ortho-phosphoric acid) in a 60:40 volume ratio. The method operated at a rate of flow 1.0 ml/min, volume of 10 µl injection, UV detection set at 260 nm, as well as an ambient temperature of 25°C, with a total runtime of 5 min. Under these conditions, Bupivacaine eluted at 2.774 min and Meloxicam at 3.494 min. System suitability parameters, including, tailing factor, plate count as well as %RSD, were within acceptable limits. The method exhibited high precision, with %RSD values below 2%, and excellent linear correlation over a range of 50-300 µg/ml for Bupivacaine as well as 1.5-9 µg/ml for Meloxicam. Sensitivity analysis determined LOD and LOQ values of Bupivacaine 0.60 µg/ml and 2.00 µg/ml, for Meloxicam 0.018µg/ml and 0.060 µg/ml respectively. Forced degradation studies showed that the method could show stability under different stress conditions, with peroxide causing the highest degradation. The validated method was applied for assay of pharmaceutical formulation confirming compliance with label claim.

Sotagliflozin is an oral antidiabetic medication that targets SGLT1 and SGLT2. This medication was not included in any pharmacopeia. The aim of this study was to develop, validate, and compare different methods for measuring the concentration of sotagliflozin in tablet form. These methods include spectro photometric techniques such as zero-order UV spectrophotometry, first-order derivative spectroscopy, second-order derivative UV spectrophotometry, and high-performance liquid chromatography (HPLC). Method A was a simple zero-order UV spectrophotometric method established for the determination of sotagliflozin in methanol at 254 nm. Method B is a first-order derivative spectrophotometric method, and method C is a second-order derivative spectrophotometric method involving the measurement of amplitudes at 264 and 234 nm, respectively. Method D was performed using HPLC, which was carried out using a C18 column mobile phase consisting of acetonitrile:0.1

The major purpose of this analysis is to develop and validate easy, economic UV-spectrophotometric method useful in the quantification of Edoxaban tosylate monohydrate in active pharmaceutical ingredients (APIs). Standard and working solutions of Edoxaban tosylate monohydrate were prepared, followed by the preparation of aliquots of working solutions at various concentrations. The method was validated by assessing key parameters, including linearity, precision, accuracy, robustness, ruggedness, and the limits of detection and quantitation. The demonstrated method has excellent linearity for Edoxaban in the concentration range of 2-24 μg/mL, with a coefficient of determination (R²) was 0.9998. This method is suitable for routine analysis of Edoxaban in bulk form, offering a reliable tool for quality control in pharmaceutical settings.

A QbD stability-indicating RP-HPLC method for posaconazole and its related substances from API’s was developed and validated. Separation was accomplished by using Box–Behnken design by varying volume of acetonitrile, pH, and flow rate. Chromatographic separation was achieved on a Zorbax SB C18 column (4.6 mm × 5.0 μm) using an gradient program consists of mobile phase A phosphate buffer and mobile phase B acetonitrile and water in the ratio (80:20

The recently approved combination of foslevodopa and foscarbidopa by the United States Food and Drug Administration provides a major advancement in treatment of Parkinson's disease. This therapy helps to maintain consistent plasma levels of levodopa, thereby minimizing overall symptom in patients. A robust and validated RP-HPLC method has been developed due to novelty of the drug combination and its recent approval by the regulatory agencies. The optimized chromatographic conditions included the use of a C18 column (250 x 4.6 mm, 5 mu m), an isocratic mobile phase of acetonitrile: 0.1% formic acid (30:70), a flow rate of 1.0 mL/min, an injection volume of 10 mu L, detection at 272 nm, and an ambient temperature of 25 degrees C, with a total runtime of 6 min. Under these conditions, foslevodopa eluted at 2.087 min and foscarbidopa at 4.166 min. System suitability parameters, including plate count, tailing factor, and %RSD, were within acceptable limits. The method exhibited high precision, with %RSD values below 2%, and excellent linearity over a concentration range of 30-180 mu g/mL for foslevodopa and 1.5-9 mu g/mL for foscarbidopa. Sensitivity analysis determined LOD and LOQ values of 0.480 and 1.700 mu g/mL for foslevodopa and 0.024 and 0.084 mu g/mL for foscarbidopa, respectively. Degradation studies confirmed the stability indicating capability of the method under various stress conditions, with oxidative stress causing the highest degradation. The validated method was applied for assay of pharmaceutical formulation confirming compliance with label claims.

Objective: In this research, a validated RP-HPLC method for analyzing teriflunomide drug substance and its associated process-related impurities was developed with the assistance of the Quality by Design (QbD) approach. Material and Method: The QbD methodology employs statistical design of experiments to establish a robust method within a defined "design space." This design space outlines the experimental parameters' range within which alterations will not significantly impact the results. Chromatographic separation was done on HPLC system connected to a PDA detector, and the column used was the C18 YmC-Triart with specifications of 125 cm x 4.0 mm x 5.0 μm. The optimized mobile phase consisted of 0.5% triethylamine buffer with pH 4.0 (± 0.05) and acetonitrile in a 65:35 v/v ratio, flow rate of 1.0 ml/min. Detection wavelength of 210 nm. Result and Discussion: The developed RP-HPLC method successfully achieved high resolution, specificity, linearity, precision, accuracy, and robustness in quantifying both teriflunomide and its impurities simultaneously. Using a design of experiments (DoE) approach, critical method parameters were systematically identified and optimized, ensuring accurate and precise determination of impurity levels across the drug substance lifecycle. This validated method provides a thorough approach to ensuring the quality and safety of teriflunomide drug substances by delivering reliable data on impurity profiles. By applying Quality by Design (QbD) principles, not only does the method enhance understanding of the analytical process, but it also supports ongoing improvement and lifecycle management of the procedure.

This study aimed to develop a stability-indicating RP-HPLC assay method for eliglustat and its organic impurities using a central composite design approach. The chromatographic separation was achieved with a 10 mM phosphate buffer at pH 4.0 on a Thermo Accucore C18 column (150 x 4.6 mm, 2.6 mu m) at a wavelength of 210 nm. Gradient elution was performed using a mobile phase-A consisting of buffer and acetonitrile in a 90:10 v/v ratio and a mobile phase-B composed of water and acetonitrile in a 35:65 v/v ratio, at a flow rate of 1.1 mL/min at 45 degrees C for a total run time of 55 minutes. Based on preliminary experiments, central composite design was utilized to evaluate the effects of independent variables such as flow rate, acetonitrile ratio and column oven temperature on the response factors. Eliglustat and its impurities (EGS-5A, EGS-Diastereomers, and EGS-N-Oxide) had retention time of 3.5 minutes, 21.5 minutes, 23.2 minutes and 25.9 minutes, respectively. The limits of detection and quantitation for eliglustat and its impurities were established in relation to the test concentration, achieving a desirability of 1. The developed method was validated as per regulatory guidelines and successfully applied in bulk drugs and formulation.

Excellent characteristics of carbon fiber-reinforced polymer (CFRP) include light weight, high strength, high modulus, and high temperature resistance. CFRP has a wide range of potential applications in the domains of public safety, aviation, and high-end non-military people products. Different methods have been used to modify the CFRP in order to increase surface action, harshness, and wettability, improving the interfacial binding between the fiber and network for better mechanical properties. Finally, a few CFRP-related difficulties are looked at, and future directions in interfacial support research are predicted. In this day and age, innovation-focused applications are becoming more significant, and the use of mechanical cycles is progressing swiftly and steadily. Due to their exceptional performance, such as low weight, high specific strength, and high specific stiffness, carbon fiber-reinforced polymer (CFRP) composites have a wide application viewpoint in the aerospace, military, and wind power sector high-quality civilian products. Currently, there is still a significant discrepancy between the theoretical calculation of the CFRP and the actual force. Improving the interface rationally is the key to solving this fundamental issue. The development, properties, and contemporary applications of CFRP composite materials, as well as their processing and boring activities, are discussed in this overview along with recent innovations and potential future applications.

Objective: For the measurement of lamivudine(LAM) and effavirenz (EVZ) in combination formulation, a uncomplicated and reliable liquid chromatographic approach has been proposed. Material and Method: Multivariate optimization of the RP-HPLC method, experimental conditions were accomplished using the design of experiments (DoE). The crucial method parameters were determined by a risk assessment. The mathematical models were created using three independent variables: percentage of acetonitrile, percentage of methanol, and buffer pH. The impacts of these independent elements were thoroughly investigated using the central composite design (CCD), which was utilized to analyze the response surface methodology. Result and Discussion: The LAM and EVZ retention time and resolution were both concurrently optimized using the desirability function. Acetonitrile, methanol, and phosphate buffer (pH 7.0) in the proportions of 40:20:40 v/v each were used in the optimized and anticipated data from the contour diagram, with detection occurring at a wavelength of 215 nm. Baseline separation of both pharmaceuticals with high resolution and a run time of under 6 minutes was accomplished under these ideal conditions. The validated test parameters followed ICH recommendations. As a consequence, the findings demonstrated that the Quality by Design methodology could be successfully used to optimize the RP-HPLC technique for the concurrent quantification of LAM and EVZ.

The current studies entail Quality by Design (QbD)-enabled development of a simple, rapid, sensitive and cost-effective high-performance liquid chromatographic method for estimation of emtricitabine (EMT), tenofovir diproxil fumarate (TEN), and efavirenz (EFA) in combined dosage form. Systematic optimization was performed employing Box-Behnken design by selecting the flow rate, buffer molarity, and acetonitrile volume as the critical method parameters (CMPs) identified from screening studies, thus evaluating the critical analytical attributes (CAAs), namely, retention duration, theoretical plates, resolution, and asymmetry factor as the parameters of method robustness. The optimal chromatographic separation was achieved using acetonitrile and phosphate buffer (pH 3.0) 74.1:25.9 v/v as the mobile phase with a flow rate 0.91 mL/min, and UV detection at 260 nm. The method was validated as per the ICH recommended conditions, which revealed high degree of linearity, accuracy, precision, sensitivity and robustness over the existing liquid chromatographic methods of the drug. Studies on forced degradation under acid, basic, oxidative, photolytic, and thermal conditions revealed the drug’s well-resolved peak and the degradation products’ peaks as well.

A simple, accurate, precise and robust reverse phase high performance liquid chromatographic (RP-HPLC) method was developed and validated for the simultaneous estimation of Bilastine and Monteleukast Sodium in bulk and pharmaceutical dosage form. Chromatographic separation was performed on an Zodiac sil RP C18 column (100mm × 4.6mm, 3µm) with mobile phase consist a mixture of 75:25% v/v acetonitrile: phosphate Buffer pH adjusted to 5.2 with ortho-phosphoric acid in an isocratic elution mode, at a flow rate of 1 ml/min. The detection was monitored at 272nm. The retention time of Monteleukast Sodium and Bilastine were found to be 3.668 min and 2.746 min respectively. Linearity range was found between 20-100µg/ml for Bilastine with correlation coefficient of 0.999 and 5-25µg/ml for Monteleukast Sodium with correlation coefficient of 0.999. This method was validated with respect to linearity, precision, accuracy, ruggedness, limit of detection, limit of quantification and robustness. This method was successfully applied for the simultaneous estimation of Bilastine and Monteleukast Sodium in bulk and pharmaceutical formulation.

An analytical method based on reverse phase-high performance liquid chromatography (RP-HPLC) has been developed and subsequently validated, which was found to be simple and rapid for the simultaneous quantification of azelnidipine and telmisartan in pharmaceutical dosage form. The separation was performed on an Intersil C18 column (250 × 4.6mm, i.d., 5µm) utilizing the mobile phase having composition 70 volumes of acetonitrile and 30 volumes of 5 millimolar phosphate buffer pH 4.6. The chromatographic analysis was carried on isocratic elution at a flow rate of 1mL/min. Detection was carried out with UV detector at 255nm, and linearity was found at concentration ranges of 10-50µg/ml for AZL and 20-100µg/ml for TEL. The recoveries obtained were 99.48‒100.22% for AZL, and 99.62 – 99.88% for TEL. No interference was found by the excipients in the formulation. The method was validated as per guidelines framed by International conference of harmonization for the parameter accuracy, precision, specificity, robustness, limits of detection and quantitation. The developed RP-HPLC method was applied in the analysis of commercial pharmaceutical products containing AZL and TEL and found to be efficient from recovery results.

The International Council for Harmonization (ICH) has classified methanol and toluene as class-2 solvents, whose use must be limited as they may cause irreversible toxicity. A simple validated Head Space Gas Chromatographic (HSGC) method using flame ionization detector was developed for determination of azeotropic residual solvent; methanol and toluene in teriflunomide drug substance. The column DB-624 with specifications (30m X 0.53mm X 3.0 μm) was used. The flow rate of nitrogen carrier gas was 2.0 mL/min with analysis run time of 26 minutes. The HSGC conditions were optimized for determination of residual screening for methanol and toluene in the drug substance. The linearity were assessed for methanol and toluene mixture from 0.65–180 μg/mL and 0.24 –54 μg/mL respectively. The limit of detection for methanol and toluene were 5.5 ppm and 2.0 ppm and limit of quantification for methanol and toluene were 16.3 ppm and 6.0 ppm respectively. The solution stability study indicated that there was no significant variation in the ppm levels of specified solvents up to 48 hours at room temperature. The ICH has limited the concentrations of class-2 solvents; methanol and toluene in pharmaceutical drug substances as 3000 ppm and 890 ppm respectively. Limit of Quantification’s for methanol and toluene in this study were satisfactory for the detection of ICH concentration limits in teriflunomide drug substance.

Chalcones are small molecules, naturally found in fruits and vegetables, and exhibit diverse pharmacological activities. They also possess anticancer activity against different tumors. They can be converted into numerous derivatives by modifying hydrogen moieties, enabling the exploration of their diverse anticancer potentials. The main aims are to provide valuable insights into the recent progress made in utilizing chalcones and their derivatives as agents against breast cancer while delivering their underlying molecular mechanisms of action. This review presents anticancer molecular mechanisms and signaling pathways modulated by chalcones. Furthermore, it helps in the understating of the precise mechanisms of action and specific molecular targets of chalcones and their synthetic derivatives for breast cancer treatment.