Bulk Form Research Articles

Understanding How the Suppression of Insertion-Induced Phase Transitions Leads to Fast Charging in Nanoscale LixMoO2.

Fast-charging Li-ion batteries are technologically important for the electrification of transportation and the implementation of grid-scale storage, and additional fundamental understanding of high-rate insertion reactions is necessary to overcome current rate limitations. In particular, phase transformations during ion insertion have been hypothesized to slow charging. Nanoscale materials with modified transformation behavior often show much faster kinetics, but the mechanism for these changes and their specific contribution to fast-charging remain poorly understood. In this work, we combine operando synchrotron X-ray diffraction with electrochemical kinetics analyses to illustrate how nanoscale crystal size leads to suppression of first-order insertion-induced phase transitions and their negative kinetic effects in MoO2, a tunnel structure host material. In electrodes made with micrometer-scale particles, large first-order phase transitions during cycling lower capacity, slow charge storage, and decrease cycle life. In medium-sized nanoporous MoO2, the phase transitions remain first-order, but show a considerably smaller miscibility gap and shorter two-phase coexistence region. Finally, in small MoO2 nanocrystals, the structural evolution during lithiation becomes entirely single-phase/solid-solution. For all nanostructured materials, the changes to the phase transition dynamics lead to dramatic improvements in capacity, rate capability, and cycle life. This work highlights the continuous evolution from a kinetically hindered battery material in bulk form to a fast-charging, pseudocapacitive material through nanoscale size effects. As such, it provides key insight into how phase transitions can be effectively controlled using nanoscale size and emphasizes the importance of these structural dynamics to the fast rate capability observed in nanostructured electrode materials.

RP-HPLC Method Validation for Levomilnacipran Estimation in Bulk and Formulation

RP-HPLC was used to build sensitive and accurate procedures for establishing and verifying analytical methods for estimating levomilnacipran in bulk and pharmaceutical dose forms. The ratio of methanol to 10 mM dipotassium hydrogen phosphate buffer pH 6.5 in the mobile phase is 50:50 (v/v%). The working standard solution was 20 g/mL. With a flow rate of 1-mL/minutes, an injection volume of 20 μL, a run time of 10 minutes, and a detection wavelength of 215 nm, the analysis was carried out on XBridgeTM C18 column 5 (250 x 4.6 mm). Readings of the precision study %RSD were found to be below the 2% limit. With a r2 of 0.998, it was concluded that the strategy was linear. The results showed that the levomilnacipran LoD and LoQ values were 1.42 and 4.75 μg/mL, respectively. The approach may be used to analyse levomilnacipran bulk and pharmaceutical formulations.

Development of Novel RP-HPLC Method for Estimating Tepotinib in Bulk and Pharmaceutical Dosage Form

Objective: The study’s goal is to develop a highly appropriate, fast, precise, and validated reverse-phase high-performance liquid chromatography (RP-HPLC) approach that indicates stability for the estimation of tepotinib in pharmaceutical dosage form and bulk, in accordance with ICH recommendations. Method: The components were separated by chromatography using a Phenomenex Kinetex XB-C18 (150×4.6 mm, 5μ) column. The absorbance was measured at 272 nm, and the flow rate was 1.0 mL̸min. The International Council for Harmonisation (ICH) states that checks were made for linearity, precision, accuracy, system appropriateness, specificity, and protocol robustness. Results: Tepotinib was shown to have a retention period of 3.4 minutes. The results showed that the linearity ranged from 5 to 25 μg/mL (r2 = 0.9993), and the percentage mean recoveries for tepotinib’s accuracy and precision fell within the range of (%RSD˂ 2). It was discovered that the Limit of Detection (LoD), and Limit of Quantitation (LoQ) were, respectively, 0.429 and 1.3 μg/mL.

Impacts of E-Beam Irradiation on Polycrystalline Metals in Both Bulk and Thin Film Forms

This study aims to explore the impact of e-beam irradiation on the mechanical and structural characteristics of four different polycrystalline metals (Ni, Cr, V, and Ti), in both bulk and thin film forms. Thin metal films are fabricated using magnetron sputtering. The primary goal is to identify suitable metal candidates for growing thin films, which could serve as exit windows for e-beam accelerators. This selection is based on their properties, power dissipation capabilities, and the effects of irradiation on mechanical attributes such as hardness, ductility, defect density, and strength.For the bulk polycrystalline metal samples, a series of nanoindentation tests has been conducted before and after e-beam irradiation to investigate changes in hardness and elastic modulus. Additionally, to compare performance with the bulk samples, thin metal films are subjected to the same procedure before and after irradiation, allowing for the evaluation of film hardness, moduli, and creep properties. Results indicate that irradiated bulk samples of Ni, Cr, and V become harder, whereas Ti experiences softening. There is no significant irradiation effect on modulus for all for polycrystalline metal samples. To understand the underlying reasons behind these effects, both the fabricated metal films and bulk metal samples undergo comprehensive characterization tests for their microstructural properties, elastic behavior, and chemical composition. This involves the utilization of SEM with EDS, FESEM and AFM to analyze microstructure and surface attributes of the films, followed by X-ray diffraction to gain insight into film morphology and lattice orientation.

Sputter Grown Hexagonal WSe2@Graphite Nanoflakes for Electrochemical Energy Storage

In the pursuit of sustainable and efficient energy storage solutions, researchers have continuously explored novel materials and technologies to enhance the performance of energy storage devices. Recently, transition metal dichalcogenide (TMDCs) such as molybdenum disulfide (MoS2), molybdenum diselenides (MoSe2), and tungsten disulfide (WS2) with a honeycomb-like structure has sparked considerable interest in utilization as electrode material for supercapacitor (SCs) applications due to their unique layered structures. Generally, the small surface area of TMDCs in their bulk form restricts their practical usage in the SCs applications. Whereas TMDC in thin 2D form exhibits high surface area and flexibility to the electrode material which allows more charge storage and results in high capacitance and energy density. In the present work, high-quality tungsten diselenide (WSe2) thin film electrodes were deposited over graphite sheets (WSe2@Graphite) using DC magnetron sputtering technique at an elevated temperature of around 200 0C under the controlled argon atmosphere. The electrochemical properties of these WSe2@Graphite electrode were investigated in three electrodes configuration using 1M Na2SO4 aqueous electrolyte by recording CV, GCD, and EIS spectra. The hexagonal WSe2@graphite nanoflakes were found to exhibit an exceptionally high areal capacitance of 88.05 mF/cm2 and energy density of 7.83 µWh/cm2 at a scan rate of 5 mV/s. Further, GCD was performed, and the WSe2@graphite electrode exhibits a high areal capacitance of 37.5 mF/cm2 at the current density of 0.5 mA/cm2. The WSe2 thin film electrode shows a high energy density of 3.3 µWh/cm2 at a power density of 199.98 µW/cm2. Additionally, the WSe2@graphite thin film electrode demonstrates high cyclic stability with retaining ~ 90.33% capacitance even after 2000 consecutive GCD cycles. The obtained hexagonal nanoflakes-like morphology provides a high surface area and porous structure that helps to improve the electrochemical performance of the WSe2 thin film. The obtained results demonstrate that the WSe2@graphite thin film exhibit excellent electrochemical performance and can be utilized as a potential material for supercapacitor electrodes. Keywords- Transition metal dichalcogenide (TMDCs), tungsten diselenide (WSe2), DC magnetron sputtering, supercapacitor, and nanoflakes Figure 1

Corrosion and Protection of Synthetic Intermetallic Compounds and Bulk Aluminum Alloy Under Simulated Atmospheric Conditions

Aluminum alloy 7075-D6 is often used for aircraft parts and is thus exposed to atmospheric conditions. AA7075-D6 is susceptible to corrosion due to high Zn, Mg and Cu contents in the form of various intermetallic particles having more or less noble electrochemical potential regarding the matrix (1,2). Usually, corrosion of aluminum alloys is simulated using solutions of various concentrations of chloride ions. However, aircraft are exposed to atmospheric conditions, where Cl- is not the only pollutant. Namely, in industrial and urban areas, major inorganic species such as ammonium (NH4 +), sulfate (SO4 2−) and nitrate (NO3 −) ions are found in the form of NH4NO3 and (NH4)2SO4 (or NH4HSO4). Therefore, these should also be considered because they represent corrosive agents for many aluminum alloys (3). Corrosive conditions may be thus better simulated by the so-called dilute Harrisonʼs solution (DHS) (0.35 wt.% (NH4)2SO4 + 0.05 wt.% NaCl), which in addition to Cl− also contains SO4 2− and nitrate NO3 − reflecting the environmental and atmospheric conditions. The first part of our study was focused on the corrosion of AA7075-T6 in DHS and comparison with NaCl solution. In addition to AA7075-T6, major intermetallic compounds (IMCs) synthesized in bulk form to represent the major intermetallic constituents (Al2Cu, Al2CuMg, Al7Cu2Fe and MgZn2) were also investigated. For IMCs, electrochemical measurements were performed using a microcell, and a standard cell was used to study the bulk alloy.Bulk AA7075-T6 was less susceptible to corrosion in DHS than in chloride solution stemming from the beneficial presence of sulfate ions and lower chloride concentration. The susceptibility of IMCs to corrosion in DHS increased as Al2Cu < Al7Cu2Fe < Al2CuMg < MgZn2 due to the increased dissolution of Mg in the presence of ammonium ions. The relative nobility of IMCs was determined based on the galvanic current density.In the second part of our study, we addressed the role of cerium salts in the corrosion protection of AA7075-T6 in DHS. Cerium salts are non-toxic compounds and demonstrate corrosion inhibition by inhibiting redox reactions by forming a protective cerium-containing precipitated conversion layer (4). Ce salts acted as inhibitors for the alloy during 14-day testing, forming a Ce hydroxide layer. The degree of protection depended on the type of anion, being the highest for Ce acetate. For the IMC, however, inhibition by Ce salts did not occur during short measurements, indicating the importance of galvanic interaction with the alloy matrix in the inhibition, which was confirmed by long-term measurements of the alloy. Micro and macro approaches give essential information on the galvanic relation between the IMPs and Al matrix under different conditions in the presence and absence of different cerium salts or other inhibitions (5). This brought about valuable information concerning corrosion inhibition and synergism with other ions in the corrosion media. Figure. Schematic presentation of (a) effect of various anions (NH4 +, SO4 2 - and Cl-) in dilute Harrison’s solution, and (b) effect of cerium(III) cations and corresponding anions (Cl-, NO3 - and CH3COO-) on the surface of AA7075-T6. Corrosion inhibition due to the deposition of the cerium layer is presented in (c). The precipitation of Ce species proceeds mainly on the cathodic sites and progressively spreads over the alloy surface; meanwhile, the Mg and Al are slowly dissolved from the anodic sites.

A Comprehensive Ecotoxicity Study of Molybdenum Disulfide Nanosheets versus Bulk form in Soil Organisms.

The increasing use of molybdenum disulfide (MoS2) nanoparticles (NPs) raises concerns regarding their accumulation in soil ecosystems, with limited studies on their impact on soil organisms. Study aim: To unravel the effects of MoS2 nanosheets (two-dimensional (2D) MoS2 NPs) and bulk MoS2 (156, 313, 625, 1250, 2500 mg/kg) on Enchytraeus crypticus and Folsomia candida. The organisms' survival and avoidance behavior remained unaffected by both forms, while reproduction and DNA integrity were impacted. For E. crypticus, the individual endpoint reproduction was more sensitive, increasing at lower concentrations of bulk MoS2 and decreasing at higher ones and at 625 mg/kg of 2D MoS2 NPs. For F. candida, the molecular endpoint DNA integrity was more impacted: 2500 mg/kg of bulk MoS2 induced DNA damage after 2 days, with all concentrations inducing damage by day 7. 2D MoS2 NPs induced DNA damage at 156 and 2500 mg/kg after 2 days, and at 1250 and 2500 mg/kg after 7 days. Despite affecting the same endpoints, bulk MoS2 induced more effects than 2D MoS2 NPs. Indeed, 2D MoS2 NPs only inhibited E. crypticus reproduction at 625 mg/kg and induced fewer (F. candida) or no effects (E. crypticus) on DNA integrity. This study highlights the different responses of terrestrial organisms to 2D MoS2 NPs versus bulk MoS2, reinforcing the importance of risk assessment when considering both forms.

Reduced toxic effects of nano‑copper sulfate in comparison of bulk CuSO4 on biochemical parameters in the Rohu (Labeo rohita)

Considering the wide application of nanoparticles in various fields of life and growing concern regarding their toxic effects, the present study was designed with the aim to evaluate the potential risks of using copper sulfate nanoparticles (CuSO4-NPs) in comparison to bulk form. Nanoparticles of CuSO4, having mean size of 73 nm were prepared by ball milling method, and fingerlings of Labeo rohita were exposed to two levels, 20 and 100 μg L−1 of CuSO4 in both bulk and nano forms for 28 days and their comparative effects on the metallothioneins (MTs), heat shock proteins 70 (HSP 70), lipid profile, cholesterol (CHOL) and triglyceraldehyde (TG) levels, activities of some metabolic enzymes Alanine transaminase (ALT), Aspartate transaminase (AST) Akaline phosphatase (ALP), and genes expressions of HSP-70, TNF-α and IL1-ß were investigated. CuSO4 showed the concentration and particle type dependent effects. The over expression of HSPs and MTs, significant decreases in CHOL, TG, low density lipid (LDL) levels and ALP activity, while significant increases in high density lipid (HDL)level as well as ALT and AST activities and HSP-70, TNF-α and IL1-β expressions were observed in response to higher concentration of both bulk and nano form of copper sulfate. At lower concentration (20 μg L−1), however, only bulk form showed toxicity. Thus, low concentrations of CuSO4-NPs pose negligible threat to freshwater fish.

UV Spectrophotometric Method for Estimation of Voriconazole in Bulk Form

This study presents a validated UV spectrophotometric method for the precise estimation of voriconazole in bulk formulations. Voriconazole, an essential antifungal agent, demands accurate quantification for its pharmaceutical applications. The proposed method leverages the sensitivity of UV spectroscopy to determine voriconazole concentrations effectively.&#x0D; The method's validation adheres to regulatory guidelines, ensuring reliability and accuracy. Spectrophotometric analysis was performed within a specific wavelength range, demonstrating linearity, precision, accuracy, and robustness across different concentrations of voriconazole.&#x0D; Parameters such as specificity, sensitivity, and stability were evaluated to affirm the method's suitability for routine analysis.&#x0D; The results indicate the method's efficacy in quantifying voriconazole in bulk and semi-solid forms with high precision and sensitivity. This validated UV spectrophotometric method presents a valuable tool for pharmaceutical analysis, facilitating quality control and assurance in voriconazole formulations.&#x0D; Keywords: Voriconazole, UV spectrophotometry, Anti-fungal, semi-solid formulation, Beer’s Lambert’s law.

A New Method Development and Validation of 5α Reductase Inhibitor (Dutasteride) Using R-HPLC In Bulk and Pharmaceutical Dosage Form (Dexamethasone Use as An Internal Standard)

The proposed HPLC Method was found to be simple,precise,accurate and economicalfor the estimation of dutasteride in Bulk and tablet dosage form. The present work, developed HPLC method was found suitable and validated. Luna – C-18 (250 mm x 4.6 mm, 20 µL) column was used for the assay. Mobile phase was Acetonitrile and Water in the ratio 80:20. Linearity was established in the range of 5-100 µg/ml with a coefficient correlation of 0.9998 and eluents were monitored at 242 nm and at 1 ml/min. flow rate. The Retention time was found to be 5.9 min. The efficiency of the column, expressed as the number of theoretical plates for six replicate injections was 11566 ± 119.695 (%CV1.03%) and USP tailing factor was 1.25 ± 0.012 (%CV 0.79). The regression equation for the calibration plot was Y = 0.0618 X – 0.008. Intra-day precision from 0.166 to 1.449 and Inter-day precision from 0.186 to 1.449. The% recovery of dutasteride from API and dosage form were 100.70% and 99.66%. The drug was subjected to stress conditions such as Oxidative and Photodegradation, Considerable degradation was found to occure in acidic and basic medium on heating at 100°C but no degradation was observed at room temperature. The drug was exposed to 10% H2O2{heating at 100°C forming degradation product at RT: 2.557}. The LOD and LOQ was 0.257µg and 0.779 µg respectively.When the flow rate was reduced, the retention time of dutasteride increased.The assay result with analyst #1 and Analyst #2 were % Assay = 98.40% (%RSD = 0.13%) and % Assay = 99.07% (%RSD =0.53) respectively. Robustness and ruggednesswasobserved that results were well within acceptance limits of 98–102%, with %RSD ±2.0%, indicating the method is rugged and provides consistent and reliable results which are not affected by small changes in experimental conditions. This method can be used for routine analysis of dutasteride. Running Title: A New Method Development and Validation of 5α-Reductase inhibitor using R-HPLC.

Ligand-based magnetic extraction and safety assessment of zinc oxide nanoparticles in food products

Zinc oxide (ZnO) is a zinc supplement widely used in health products and is approved by the FDA as Generally Regarded as Safe (GRAS). However, concerns have arisen regarding the potential health effects of nanoscale ZnO, as its reactivity differs from that of its bulk form. This has led to the need for an efficient method to extract ZnO from food products without altering its physicochemical properties, where conventional methods have proven to be inadequate. This study introduces an innovative approach using starch magnetic particles (SMPs) functionalized with a 12-amino acid peptide modified with five lysines (ZBP), that has specific affinity to ZnO. ZBP@SMPs effectively and rapidly extract intact ZnO from food products, achieving recovery efficiencies ranging from 60% to 90%, all while maintaining its morphology and crystallinity. The diameter of ZnO particles recovered from six commercial food products ranged from 25 to 500 nm, with 33% falling below 100 nm, highlighting the need for a size-dependent toxicity study. However, cytotoxicity assessment on human intestinal Caco-2 cells shows all ZnO samples affects cell proliferation and membrane integrity in a dose-dependent manner due to partial dissolution. This study contributes to understanding the safety of ZnO-containing food products and highlights potential health implications associated with their consumption.

Development and Validation of RP-HPLC method for the estimation of Plecanatide from Bulk and Pharmaceutical Dosage form

A novel, simple, efficient, rapid, and precise reverse-phase high-performance liquid chromatography (RP-HPLC) method was developed for the estimation of Plecanatide in the bulk and pharmaceutical dosage form. The currently developed method was subsequently validated according to ICH guidelines in terms of linearity, accuracy, precision, the limit of detection, the limit of quantification, robustness, etc. The separation of the selected drugs was optimized after several trials including change of mobile phase and its composition, stationary phase, flow rate, column temperature, etc. The separation was performed by using an Develosil ODS HG-5 and UV absorption was measured at 246 nm. Ortho phosphoric acid, Triethylamine buffer : Methanol [520 : 480] was selected as the mobile phase at a flow rate of 1 mL/min. As per International Conference on Harmonization (ICH) Q2 R1 guidelines, several validation parameters were evaluated which include specificity, linearity, precision, accuracy, the limit of detection (LOD), and the limit of quantitation (LOQ). The acceptable degree of linearity range was found to be 10 to 60 µg/mL. The percent recovery was found to be 98.55 to 101.88%. Hence, the proposed method is simple, selective, and specifically meets the requirements of ICH guidelines for the validation of the analytical method.

Orchestrating the impact of antisites and vacancy defects on the elastic and optoelectronic properties of boron arsenide.

Cubic boron arsenide (c-BAs), a semiconducting material with ultra-high thermal conductivity and carrier mobilities, has been studied using first-principles calculation. This study examined the elastic and optoelectronic properties of c-BAs. The challenge of subphase boron (B) formation in bulk form owing to the volatile nature of arsenic (As) makes it mandatory to calculate its optoelectronic properties, by producing vacancies and antisite defects with BAs (As atom on a B site) and AsB (B atom on an As site). The mechanical properties including bulk (B), shear (G) moduli, and Poison's ratio of all the systems were studied. It was found that mechanical instability of the structure is observed for the overall vacancy creation, arsenic substitution, and mutual antisite defects. Further, pristine c-BAs showed an indirect bandgap of 1.48eV. Defect formation reduces the bandgap and shifts the absorption peaks, which improves the overall optoelectronic properties of the host material. In addition, B vacancy formation shows the maximum optical absorption and reflectivity and low energy loss, suggesting its potential applications for optoelectronic devices. The obtained anticipated data from this study is for the optoelectronic and elastic properties of c-BAs, for the device applications in photonics and electronics. In this paper, the elastic and optoelectronic properties of the pristine and defected c-BAs were systematically investigated using the Spanish Initiative for Electronic Simulations with Thousands of Atoms (SIESTA). The SIESTA program uses pseudopotentials in the norm-conserving nonlocal forms and pseudo-atomic orbital (PAO) basis set with a double-zeta potential (DZP) which are fundamental for calculating the Hamiltonian and overlap matrices in O(N) operations.

Nano-liposome of thyme essential oil promotes growth performance, antioxidant and immune responses to aeromonad septicemia in Nile tilapia, Oreochromis niloticus, fingerlings

Nano-encapsulation protects essential oils and increases their efficiency, compared to bulk forms. Hence in the present study, four diets (328 g/kg crude protein and 4402 kcal/kg gross energy) containing 0 (CTL), 25 mg/kg (25TV), 50 mg/kg (50TV), and 100 mg/kg (100TV) thyme, Thymus vulgaris, essential oil nano-liposomes (TV-NP) were offered to Nile tilapia fingerlings (initial weight of 4.27 ± 0.05 g) at water temperature of 26.46 ± 0.43°C, followed by intraperitoneal infection by Aeromonas hydrophila. Three hundred and sixty healthy fish were stocked in 12 tanks (60 L), 30 fish per tank, with daily water renewal rate of 40%. Each diet was offered to three tanks for 70 days. The fish were sampled at the end of feeding period and 12 h after the bacterial challenge. Compared to CTL, 50TV and 100TV treatments exhibited significant elevations in growth rate (14-17%; P&amp;lt;0.001), intestinal activities of amylase (9-19%; P=0.004), lipase (13-26%; P&amp;lt;0.001), protease (20-23%; P=0.001), and post-challenge survival (26-27%; P=0.001). Plasma lysozyme (14-15% P&amp;lt;0.001) and complement (5.1-5.4%; P=0.004) activities significantly increased in 25TV and 50TV, but decreased (lysozyme: 19%, complement 5.9%) in 100TV before the challenge; however, all TV-NP treatments showed similar lysozyme and complement activities after the challenge that were higher than CTL. 50TV and 100TV treatments also showed a decrease in lipid peroxidation (23-26%; P&amp;lt;0.001) and highest glutathione peroxidase activity (17-18%; P=0.001) and pre-challenge superoxide dismutase (21%; P=0.046) and catalase (15-17%; P=0.001) activities. Expression of tumor necrosis factor-alpha (11-fold, P&amp;lt;0.001), inerleukin-1 beta (5-fold, P&amp;lt;0.001), and transforming growth factor-beta (31-fold; P=0.001) in head kidney significantly increased in 100TV before the challenge. After the challenge, the transcripts of the cytokines significantly increased in all treatments and the highest expressions were observed in 50TV and 100TV treatments (62-148-fold). In conclusion, dietary 50-100 mg/kg TV-NP can be considered as a new feed additive in tilapia culture, as it improves growth rate, antioxidant capacity, and disease resistance in the fish.

Quality by design optimization and validation of a HPTLC-MS method for simultaneous estimation of paracetamol and prochlorperazine from bulk and formulation

Study reports that the, stability indicating high-performance thin layer chromatographic technique (HPTLC) was developed as well as validated for estimating Paracetamol and Prochlorperazine in bulk and dosage form. These drugs are largely used in migraine and first line treatment of schizophrenia. Selected drug combination employed for Quality by design based Box Behnken design by high performance thin layer chromatography method utilizing aluminium plates; pre-coated using silica gel 60F254 as stationary phase by using acetone: toluene: methanol (4:4:2 v/v/v) as a mobile phase. Densitogram shows Rf values for Paracetamol at 0.74 and for Prochlorperazine at 0.32 evaluated by densitometry measurement bands at 248 nm. Paracetamol and Prochlorperazine marketed formulation of 700 mg by using various excipients prepared at lab scale and it was evaluated for various types of tablet tests, and it showed the accurate result with respect to standard guidelines. The approach has been validated in accordance with International Conference on Harmonization (ICH) requirements. The correlation coefficient was found to be 0.992 and 0.998 at a concentration range of 100–300 μg/band and 1000–3000 ng/band for Paracetamol and Prochlorperazine, respectively. The method had an accuracy of 100.51 % and 100.53 % for Paracetamol and Prochlorperazine, respectively. The degradation of Paracetamol and Prochlorperazine was carried out in an acid, alkaline, oxidative, thermal and photolytic environment. The stress degraded product was successfully separated using the HPTLC and using high resonance mass spectroscopy technique (HRMS-MS), the degradation product was discovered.

A New Colorimetric Development and Validation of Visible Method for Estimation of Atorvastatin in Bulk Formulation

A simple, sensitive, accurate, precise and economical visible Spectrophotometric method was developed and validated for the estimation of Atorvastatin in Bulk form. The method is based on the reaction of Atorvastatin with MBTH Reagent [3-Methyl-2-Benzothiazolinone Hydrazone] in the presence of ferric chloride giving greenish blue colour chromogen which shows maximum absorbance at 566nm against reagent blank. The Chromogen obeyed Beer’s law in the concentration range of 5-25 µg/ml for Atorvastatin. The results of the analysis have been validated statistically and recovery studies confirmed the accuracy of the proposed method.

Development of Visible Spectrophotometric Method and its Validation for Dolutegravir in Tablet Dosage Form

Objective: There are several methods for analyzing the same, however, they are time-consuming and costly. We created a new spectrophotometric method for determining Dolutegravir (DLT) in tablet dosage forms that is simple, accurate, and precise. We developed and validated a simple, accurate, and precise colorimetric method for the quantitative analysis of Dolutegravir in bulk and dosage form by ICH recommendations in this study. Methodology: There are several methods for analyzing the same, however, they are time-consuming and costly. We created a new spectrophotometric method for determining Dolutegravir (DLT) in tablet dosage forms that is simple, accurate, and precise. In methanol, the initial stock solution of Dolutegravir was prepared. The method is based on the formation of a blue color chromogen complex from Dolutegravir oxidation-reduction with Ferric chloride in the presence of potassium ferricyanide. Result: The color complex was measured at 710nm. Beers law was observedin the concentration range of 3.5-6.5μg/ml witha coefficient of correlation (R2) was 0.998. The system suitability criteria were found to be within the limits. The LOD and LOQ were found to be 0.91 and 2.47, indicating that the method is sensitive. Conclusion: The relative standard deviation (RSD) and percent recovery values were found to be satisfactory, indicating that the proposed method is suitable, accurate, and precise and that it can be used in routine analysis of Dolutegravir in tablet dosage forms, with relatively low-cost solvents.

Stability Indicating HPTLC Method Development and Validation for Acebrophylline in Bulk and its Tablet Dosage Form

A simple, precise, accurate stability-indicating method was developed and validated for Acebrophylline in bulk and tablet dosage form. The chromatographic separation was achieved by using Methanol: Acetonitrile: Acetone: Formic acid (4:4:2:0.1 v/v/v/v) as mobile phase and UV detection at 272nm. The retention factor for Acebrophylline was found to be 0.74±0.10. The developed method was validated with respect to linearity, accuracy, precision, limit of detection, limit of quantitation, and robustness as per ICH guidelines. Results were found to be linear in the concentration range of 400-2400ng band -1 with a correlation coefficient of 0.9921. The % assay was found to be 102.4±5. The drug was subjected to stress conditions of hydrolysis (acid, base), oxidation, photolysis, and thermal degradation. The developed method can be used for the quantification of drug in the dosage form, bulk drug as well as for routine analysis in quality control laboratories.

A Validated RP-HPLC Method for Simultaneous Estimation of Benidipine and Telmisartan in Bulk and Tablet Dosage Form

Background: In this work, a novel, simple and accurate reverse phase high-performance liquid chromatographic method with UV detection is presented for the simultaneous estimation of Benidipineand Telmisartan in API and marketed formulations. Objective: To develop and validate this method in accordance to regulatory guidelines i.e. ICH Q2B-R1 for analytical parameters. Methods: In RP-HPLC the separation was achieved using a Xbridge C18 (250x 4.6 i.d; 5µm) column with isocratic elution using a mobile phase consisting of methanol: acetonitrile (80:20v/v/ with 0.1% v/v TEA) adjusted to pH 5.2 with glacial acetic acid at 1mL/min flow for 10min. Benidipine and Telmisartan, were detected at dual wavelength at 237 and 297nm with retention time (Rt) 6.891 and 8.997 minutes respectively. Results: Our new methods (RP-HPLC) were found to (r2&gt;0.999) for both Benidipine and Telmisartan. The developed methods are highly selective, precise and reproducible with %RSD &lt; 2%, Moreover the methods are accurate with recovery more than 99% in both methods. Conclusion: The RP-HPLC method results are efficient, simple and easy. These highly sensitive methods were successfully applied for assay determination of both Benidipine and Telmisartan at fixed dose combination.

A validated RP-UPLC method for estimation of Samidorphan and Olanzapine in mixed powder and combined tablets

Back groundThe key objective of the research study is to develop a new stability-indicating RP-UPLC approach to determine the presence of Samidorphan and Olanzapine simultaneously in bulk and their combination. A successful separation of Samidorphan and Olanzapine was achieved by using HSS column C18 (100 × 2.1 mm), a mobile phase of 0.1% orthophospharic acid: Acetonitrile (70:30 v/v), flow rate of 0.3 mL/min, and detection wavelength of 230 nm. The stability of the analytes in bulk and dosage forms was evaluated using extreme forced conditions, such as hydrolysis with acid and base, peroxide oxidation, and heat degradation, following ICH guidelines.ResultsOlanzapine and Samidorphan had retention times of 0.46 and 0.93 min, respectively. Olanzapine and Samidorphan have linear responses from the proposed method in the concentration ranges of 5–30 µg/mL and 2.5–15 µg/mL, respectively. The computed detection and quantification limits for Olanzapine were 0.22 µg/mL and 0.471 µg/mL, and for Samidorphan were 0.12 µg/mL and 0.36 µg/mL. All method validation parameters have complied with the ICH guidelines' Q2 acceptance limits. The stability representing the feature of the approach has been seen with the excellent resolution among the Olanzapine and Samidorphan and degradation products.ConclusionThe suggested RP-UPLC method was extremely sensitive, precise, and stable-indicating. The technique can potentially be used in the production of Olanzapine and Samidorphan for routine analysis in the quality control department.Graphical abstract