Bulk Form Research Articles (Page 1)

Development and Validation of a UV Spectroscopic Method for the Estimation of Gepirone Hydrochloride in Bulk and Tablet Dosage Form in Dissolution Media

Clinical application of beta-tricalcium phosphate (β-TCP) has been limited by a lack of bone infiltration within its bulk form. Lithography-based ceramic manufacturing (LCM), a novel additive manufacturing (AM) technique, leverages photopolymerization to create β-TCP structures with higher feature resolution and surface quality than traditional techniques. This modality allows for a more efficient and precise means to control implant microarchitecture and macroarchitecture, enabling the production of novel implant configurations. This pilot study explores the bone regenerative capacity of lithography-based ceramic-manufactured 100% β-TCP scaffolds for the repair of critically sized mandibular defects in a skeletally mature rabbit model. Quantitative and qualitative analyses of regenerated bone were performed using micro-computer tomography (micro-CT) and two-dimensional histologic analysis, respectively. Three-dimensional volumetric reconstruction revealed bridging bone in sites treated with β-TCP implants, yielding ~8.6±3.5% of regenerated bone within the construct and ~33±3.2% remaining scaffold volume. Bone regeneration and remaining scaffold quantification were corroborated using traditional two-dimensional histologic micrographs and three-dimensional volumetric analysis (P<0.05). Qualitative histologic analysis revealed vascularized woven and lamellar bone, with no evidence of ectopic bone, excess inflammation, or fracture. Bone regeneration in this short-term rabbit model following a critical-sized mandibular defect repaired with LCM β-TCP scaffolds demonstrated analogous radiographic and histologic properties to native bone.

Development of an environmentally friendly RP-HPLC method for the concurrent determination of sitagliptin and metformin in bulk and tablets dosage forms using an analytical Quality by Design approach: sustainability and greenness rules for appraisal

Ecologically conscious profiles assessments for economic, and concurrent HPLC detection of chlordiazepoxide and clidinium bromide in bulk and tablets solid dosage form

This work demonstrates simple and reliable spectrophotometric methods for the simultaneous determination of paracetamol (PAR) and meloxicam (MEL) in mixture I as well as PAR and domperidone (DOM) in mixture II in bulk form and laboratory-made tablets. Successful determination of mixture I was accomplished using direct zero-order spectrophotometry at 361 nm for MEL and first-order derivative (1D) spectrophotometry by measuring the peak at 342 nm and the trough at 262 nm for MEL and PAR respectively. On the other hand, a ratio difference method was suggested for the analysis of mixture II. The difference between the ratio spectra amplitudes at 256 and 288 nm were recorded for PAR determination, and 216 and 288 nm for DOM quantitation using 50 µg/mL DOM and PAR respectively as divisors. The efficacy of the proposed procedures was assessed using ICH criteria for linearity, ranges, precision, accuracy, detection, and quantitation limits. With regard to mixture I, the calibration curves showed linearity in the ranges of 3–30 µg/mL for MEL (zero-order method) and 2.5–30 and 3–15 µg/mL for MEL and PAR, respectively (first-order method), with correlation values of at least 0.9991.Whereas for mixture II, with correlation coefficients of 0.9999, the calibration curves for PAR and DOM were linear in the ranges of 3–70 and 2.5–15 µg/mL, respectively.The established procedures were used to analyze the combinations in the lab-prepared pills, and assay results were compared with reported methods. Greenness of the devised spectrophotometric procedures was assessed using the Analytical Eco-Scale and the Analytical Greenness metric (AGREE).Supplementary InformationThe online version contains supplementary material available at 10.1186/s13065-025-01643-7.

In recent decades, g-C3N4 has emerged as a potential candidate among the 2D materials for revolutionizing the use of materials in water remediation applications. g-C3N4 is an accessible semiconductor with excellent conductivity but faces challenges in its bulk state due to fast recombination rates, few active sites for adsorption, and poor light absorption capacity. The prime focus of this work is to address these drawbacks and develop an efficient metal-free photocatalyst that only uses g-C3N4. The main aim is the engineering of metal-free, pristine g-C3N4 ultrathin nanosheets (NS) and partially exfoliated nanosheets (PS) from the bulk form via two scalable post-processing methods (thermal exfoliation and mechano-hydrothermal treatment) in the absence of dopants, heterojunctions, or co-catalysts. The engineered g-C3N4 sheets help to conduct a straight comparison between the photocatalytic enhancement that exclusively arises from different tailored morphologies, thus enabling precise benchmarking of the adsorption, charge dynamics and ROS-mediated degradation properties of different morphologies. The formed bulk g-C3N4 (BS), ultrathin nanosheets (NS) and partially exfoliated form (PS) were rigorously studied with analytical tools to understand their structure-property-activity relationships. Remarkably, NS had the highest degradation efficiency (97%) toward methylene blue dye under visible-light illumination within 60 min followed by PS (82%) and BS (62%). EPR analysis and scavenging test showed that super oxide radicals and singlet oxygen are responsible for the enhanced and rapid degradation of MB. The intermediates involved in MB breakdown and the degradation pathway were outlined through LC-MS studies. Experimental UV-Vis DRS analysis was correlated with DFT calculated bandgaps, thus enabling a rare dual insight into band structure evolution. In addition, a clear quantitative relationship was recognized between the surface area, porosity and degradation efficiency. The developed photocatalysts demonstrated excellent stability over six cycles of reuse, and were used in the degradation of a complex water matrix with a mixture of various dyes, where an outcome of 80.9% mineralization emphasizes their practical relevance. The use of plant growth (green gram seeds) as a proxy for toxicity suggested that the growth rate (root length 16 cm; shoot length 14 cm) is similar for plants grown using distilled water and dye-containing water treated with the NS photocatalyst, further substantiating the environmental sustainability of the catalyst. This research underlines the potential of morphology controlled, metal-free, scalable g-C3N4 as an excellent green photocatalyst for sustainable water treatment.

Present study deals with simultaneous determination of Tolperisone and Etoricoxib in their binary mixture and their tablet dosage form by UV-VIS spectrophotometry based on the additivity of absorbance of drugs. The drugs show maximum absorbance at 255 nm (λ1) for Tolperisone and 275 nm (λ2) for Etoricoxib in methanol so these wavelengths were selected for further analysis by simultaneous equation method. For absorbance ratio method 245 nm was selected as λ1 (isobestic point) and 275 nm as λ2. Matrix was drawn using the standard absorptivity values obtained at both wavelengths, the amount of drug in the sample was calculated by solving matrix using simultaneous equation method and absorbance ratio method. Also, estimation was done by first derivative spectroscopy method where estimation of drugs was carried at zero crossing point of other drug. Drugs obey the Beers-Lambert’s law at these selected wavelengths of maximum and found to be linear in the range of 5-30 µg/mL for Tolperisone while 2-12 µg/mL for Etoricoxib. The developed methods were validated as per ICH guidelines. The precision was carried out at two level viz intra-day and inter-day for which the RSD was found within limit (&lt;%2). Recovery study was carried out on the developed method and the recovery was found to be in the range of 99.0 – 101.0 %. Methods were found to be simple, sensitive, precise and accurate. The developed methods can be applied for the routine analysis of the Tolperisone and Etoricoxib in bulk and their formulation.

2D van der Waals (vdW) ferroelectrics have aroused great interest for their novel structures and functionalities in many applications such as in-memory computing and ferroelectric detectors. However, the documented 2D ferroelectrics remain very rare, mainly limited to inorganic ones represented by transition metal thio/selenophosphates. Constructing new 2D vdW ferroelectric categories may bring interesting phenomena, but it has always been a challenge. Here, a molecular 2D vdW ferroelectric sodium 2,2,3,3-tetrafluoropropionate (2,2,3,3-TFPS) is successfully designed through H/F substitution, which adopts a unique stable layered structure where each coordination bonded molecule-based 2,2,3,3-TFPS monolayers knitted together by weak vdW forces between protruding (-CHF2) cantilevers in the adjacent two monolayers. More strikingly, it can show robust room-temperature ferroelectricity even in a mechanically exfoliated ultrathin flake as thin as 9nm, which has never been achieved in traditional molecular ferroelectrics with ferroelectricity mainly in the bulk form and micron-scale thin film. To the best of the knowledge, 2,2,3,3-TFPS is the first molecular 2D vdWs ferroelectric showing robust ferroelectricity in sub-10nm thickness. This work expands the diversity of 2D vdW ferroelectrics and sheds light on the exploration of molecular 2D vdW ferroelectrics with promising low-dimensional ferroelectricity for applications in nanoscale devices.

The study was aimed to create and verify a new, straight-forward, accurate, and specific UV-Spectrophotometric analysis method of dasatinib, by comparing in-between three different types of body fluids, having three different pH, like a) gastric fluid, b) physiological fluid c) intestinal fluid, and to determine the best suitable site for administration also. UV spectrophotometric analysis was carried out by utilizing a Shimadzu UV-visible spectrophotometer. The spectrum of the reference solution was run in the 200–400nm range. nm range in order to figure out the absorption maximum (λmax) of dasatinib, which was discovered at 323nm. The standard solution’s absorbance of 2,4,6,8 and 10μg/mL was determined the solution of 323nm against the blank. And then the three plots were compared among themselves. Gastric fluid, having a pH value of 1.2, was found to be the best option for determining by the UV spectrophotometry method. The drug dasatinib was best soluble in pH 1.2 buffer as compared with pH 7.4 and 6.8 buffers. In the suggested UV visible spectrophotometry, ICH criteria were followed, and the findings and statistical parameters showed that the development technique was sensitive, exact, and easy to use for dasatinib estimation in bulk form.

The study was aimed to create and verify a new, straight-forward, accurate, and specific UV-Spectrophotometric analysis method of chlorzoxazone, by comparing in-between three different types of body fluids, having three different pH, like a) gastric fluid, b) physiological fluid c) intestinal fluid, and to determine the best suitable site for administration also. UV spectrophotometric analysis was carried out by utilizing a Shimadzu UV-visible spectrophotometer. The spectrum of the reference solution was run in the 200–400 nm range in order to figure out the absorption maximum (λmax) of chloroxazone, which was discovered at 232 nm. The standard solution’s absorbance of 5,10,15,20,25,30 and 35 μg/ml was determined the solution of 232 nm against the blank. And then the three plots were compared among themselves. Intestinal fluid, having a pH value of 6.8, was found to be the best option for determining by the UV spectrophotometry method. The drug chlorzoxazone was best soluble in pH 6.8 buffer as compared with pH 7.4 and 1.2 buffers. In the suggested UV visible spectrophotometry, ICH criteria were followed, and the findings and statistical parameters showed that the development technique was sensitive, exact, and easy to use for chlorzoxazone estimation in bulk form.

Ertugliflozin, a selective sodium-glucose co-transporter 2 (SGLT2) inhibitor, is widely used for managing type 2 diabetes mellitus. The current study focuses on the development and validation of a robust, accurate, and precise Reverse Phase High-Performance Liquid Chromatography (RP-HPLC) method for the estimation of Ertugliflozin in a laboratory-prepared tablet formulation. Chromatographic separation was achieved using a Phenomenex C18 column (250mm × 4.6mm, 5µm) with an isocratic mobile phase of acetonitrile and water in the ratio of 70:30v/v, at a flow rate of 1.0mL/min and detection wavelength of 223nm. The method was validated as per ICH Q2(R1) guidelines. Linearity was established in the range of 1.0–15.0µg/mL with a correlation coefficient (R²) of 0.99997. The method demonstrated acceptable results for system suitability, accuracy (mean recovery: 99.61%), precision (intra- and inter-day %RSD &lt;2%), specificity, robustness, LOD (0.150µg/mL), and LOQ (0.455µg/mL). The method is suitable for routine analysis of Ertugliflozin in bulk and tablet dosage forms.

The objective of the present study was to develop and validate a simple, accurate, and robust reverse-phase high-performance liquid chromatographic (RP-HPLC) method for the estimation of Metoprolol Succinate in bulk drug and marketed formulations. Chromatographic separation was achieved using a Phenomenex C18 column (250 mm × 4.6mm, 5µm) with an isocratic mobile phase consisting of Methanol and 0.1% Orthophosphoric Acid in Water (60:40 v/v) at a flow rate of 1.0mL/min. The detection was carried out at 222nm using a UV detector. The method demonstrated a good retention time with a total runtime of 6 minutes. The linearity of the method was observed in the concentration range of 5–15µg/mL with a correlation coefficient (R²) of 0.99994. The accuracy of the method was confirmed with a recovery of 99.40%, and precision results showed %RSD values well within the acceptable limit (&lt;2.0%). The method also complied with ICH guidelines for parameters such as specificity, robustness, solution stability, and filter compatibility. The LOD and LOQ were calculated as 0.142µg/mL and 0.429µg/mL, respectively. Therefore, the developed RP-HPLC method is highly suitable for routine quality control analysis of Metoprolol Succinate in pharmaceutical formulations.

Metoprolol succinate (MTS) is a β1-selective adrenergic receptor blocker widely used for the treatment of hypertension, arrhythmias, heart failure, and myocardial infarction. Due to its significant therapeutic role, the accurate quantification and analysis of metoprolol succinate are essential. Various analytical methods have been developed for its estimation in bulk and pharmaceutical dosage forms, including spectroscopic and chromatographic techniques. This review explores different analytical methodologies for metoprolol succinate quantification, emphasizing spectrophotometric techniques and chromatography techniques. High-Performance Liquid Chromatography (HPLC) plays a crucial role in ensuring precise and reliable drug estimation. This review focuses on the significance of HPLC as the primary analytical technique for metoprolol succinate analysis. Among these, Reverse Phase High-Performance Liquid Chromatography (RP-HPLC) is widely preferred due to its high sensitivity, accuracy, and precision. Several validated RP-HPLC methods have been reviewed, detailing their mobile phase composition, column specifications, flow rate, detection wavelength, and validation parameters such as linearity, accuracy, precision, limit of detection (LOD), and limit of quantification (LOQ).

Abstract Germanium selenide (GeSe) is a promising layered semiconductor for optoelectronics. Its bulk form yet a comprehensive understanding of its strain-dependent electronic properties remains underdeveloped, especially compared to its monolayer counterpart. Herein, we present a systematic first-principles study on the evolution of the electronic structure of bulk GeSe under uniaxial strain applied along the zigzag and armchair directions. Like the observations in strained monolayer GeSe, we find that the value of the bandgap is effectively tunable with strain. While the relationship between the gap and the bond length d1 is highly anisotropic, our key discovery is a unified, exponential scaling law governing the bandgap evolution with the bond length d2 for both crystallographic directions. This finding identifies that d2 effectively integrates the lattice information into a single predictive parameter linked to the energy of the conduction band minimum. This work provides a fundamental scaling principle for strain engineering in bulk GeSe, offering a powerful tool for the rational design of its optoelectronic properties.

Interactive effects of Titanium-based compounds with Gadolinium and Mercury in Mytilus galloprovincialis.

Comparative analysis of bioaccumulation and biological impacts of cadmium sulfide (CdS) bulk versus nanoparticles in the freshwater snail Helisoma duryi.

DAMIU is a business entity that manages drinking water for public consumption needs in bulk form and not in bottled form. Based on the profile of the Surabaya City Health Service for 2019-2021, Tambak Wedi Community Health Center is included in the top 10 in the category of low levels of DAMIU sanitation inspection results for 3 years, namely from 2019-2021. Based on data from the Surabaya City Health Service, in 2019 53.85% did not meet the requirements. In 2020, 44.44% did not meet the requirements. In 2021, 54.44% do not meet the requirements. This research aims to determine the evaluation of the implementation of DAMIU sanitation inspections in the Tambak Wedi Health Center Work Area. This research is descriptive research using quantitative and qualitative research methods. The data obtained was then analyzed and evaluated using a management information system approach by evaluating the input, process, output and outcome variables of management sanitation inspection activities. The research results showed that the input components which included: work plans received a good category, policies received a good category. Human resources include: head of community health center in good category, sanitarian in good category, budget in good category, inspection method in good category, facilities in good category. Process components include: implementation planning obtained a good category, implementation of sanitation inspections obtained a good category, implementation results obtained a good category, employee development in the poor category, raw water processing in a good category, behavior of handlers, cleaning of gallon/outlets in a good category, periodic laboratory examinations in a good category. output component: evaluation of the implementation of inspections in the good category. The outcome component (quality of refillable drinking water) is in the poor category. So there is a need for intensity in training DAMIU employees and increasing the number of health center sanitarian personnel.

Inorganic/organic hybrid biomaterials have the potential to combine the benefits of bioactive glasses, such as bone bonding and osteogenesis, with the ability to withstand cyclic loading. Here, we report on silica/poly(ε-caprolactone-methacrylate) hybrids, using hydroxy monofunctional-PCL as a reversible addition-fragmentation chain transfer (RAFT) agent, for controlled polymerization of PCL-b-P(methyl methacrylate-co-3-(trimethoxysilyl)propyl methacrylate), PCL-b-P(MMA-co-TMSPMA), block copolymers by a combination of ring opening polymerization (ROP) and RAFT polymerization techniques. The new polymer was used for the preparation of hybrids via the sol-gel method, with TMSPMA providing covalent bonds between the silica and PCL-b-P(MMA-co-TMSPMA). The effect of the ratio of CL/silane containing units on the mechanical properties of the hybrids was investigated. The compositions that yielded optimal mechanical properties in bulk form (yield stress 39.3 MPa to 52.9 MPa at a strain of 4-6%) were developed into "inks" for 3D printing porous biodegradable scaffolds for biomedical applications by direct writing. Degradation tests of scaffolds in phosphate buffered saline (PBS) over the course of 180 days showed ∼30% degradation of PCL. The mechanical properties of scaffolds with pore channels of 234-380 μm reduced yield strength to 5.2-7.4 MPa, but yield strain remained at ∼4%. In vitro studies indicated biocompatibility, in terms of exposure of human bone marrow stem cells (hBMCs) to the dissolution products of the scaffolds.

High purity aluminum in its bulk form has intrinsicallyhigh reflectancein the far-ultraviolet (FUV) regime and finds utility in astrophysicalinstrumentation applications. However, bulk Al oxidizes rapidly inthe atmosphere, and its native oxide strongly absorbs and severelydegrades the observed FUV properties relative to bare Al. Varioustechniques have been investigated to produce coatings that inhibitaluminum oxide formation and lead to high FUV mirror reflectance.This work examines the development and use of a uniquely modified,hybrid plasma-enhanced atomic layer deposition (PEALD) system to passivatealuminum mirrors with metal fluoride films. This system combines twoplasma sources in a commercial atomic layer deposition (ALD) reactor.The first is a conventional inductively coupled plasma (ICP) sourceoperated as a remote plasma, and the second is an electron beam (e-beam)driven plasma near the mirror surface. To establish the operatingconditions for the in situ e-beam plasma source, the effects of samplegrounding, SF6/Ar flow, and sample temperature on resultingAlF3 films were investigated. Optimal operating conditionsproduced mirrors with excellent FUV reflectivity, 92% at 121 nm and42% at 103 nm wavelengths, which is comparable to state-of-the-artAlF3-based passivation coatings and matches that of previouslyreported ex situ e-beam plasma-processed mirrors. This optimized insitu e-beam process, along with XeF2 passivation, is thenexplored to produce a clean seed layer (unoxidized Al surface) forsubsequent PEALD of AlF3. Both approaches are demonstratedas valid pretreatments before PEALD of AlF3, showing apromising pathway for the deposition of other fluoride-based layers,such as MgF2 or LiF, with ALD or PEALD.

Selumetinib (SEL) is a recently approved medication for paediatric patients who have neurofibromatosis type 1. It is the first approved therapy for this rare, debilitating, and disfiguring disease. Development of proper analytical platforms for SEL analysis in its marketed pharmaceutical formulation (Koselugo® capsules) and blood plasma is highly warranted. Availability of such analytical tools would ensure SEL capsules' quality and effective therapy. This study introduces, for the first time, the development of two label-free and sensitive platforms for SEL quantification in capsules and human plasma. These platforms are microwave-assisted with an ultraviolet absorbance microplate reader (MW-UV) and reverse-phase high-performance liquid chromatography with a photodiode-array detector (HPLC-PDA). Both platforms employed the SEL native UV absorption as an analytical signal. The MW-UV measured the UV absorption in 96-well transparent plates at 255 nm. The HPLC-PDA involved chromatographic separation of SEL and tozasertib (TOZ), internal standard, on a C18 column both were detected at 255 nm. The optimum procedures of both platforms were established and validated following the ICH guidelines. The linearity ranges were 15-500 µg mL-1 and 0.8-100 µg mL-1, with limits of quantification of 15.3 and 3.5 µg mL-1, for MW-UV and HPLC-PDA, resp. Both platforms displayed high precision with relative standard deviation values ≤ 1.8 %, and high accuracy with recovery ranging from 98.3 to 102.3 %. The platforms were successfully applied to quantify SEL in bulk form, Koselugo® capsules, and were preliminarily applied to human plasma analysis. Eco-friendliness assessment confirmed the adherence of both platforms to green analytical approaches. MW-UV and HPLC-PDA are simple and fast, enabling high-throughput analysis, thus introducing valuable tools for routine use in quality control and clinical laboratories for SEL quantification.