High-performance Method Research Articles

A high-performance thin-layer chromatography densitometric method for the separation of isomeric ceftriaxone in powder for injection formulation

The aim of this study was to develop and validate a High-Performance Thin Layer Chromatographic (HPTLC) method for simultaneous determination of ceftriaxone and ceftriaxone e-isomer in powder for injection formulation. Ceftriaxone sodium injection is an antibiotic that used globally. It has Z/E geometrical conformation, in which ceftriaxone sodium and 3 ene-isomer have Z- conformation while (E)-isomer has E- conformation and the potential toxicity of ceftriaxone (E)-isomer has been reported. Thus, to safeguard the public health, a simple and easy to use, rapid and reliable method was developed for qualitative and quantitative determination of ceftriaxone sodium and its (E)–isomer. Samples were applied on HPTLC glass plates precoated with silica gel 60F254 by using Linomat semi-auto sampler. Separation was carried out using acetone, triethyl amine, water, chloroform and ethyl acetate as a mobile phase in different ratios. The Rf values of separated compounds were 0.51 ± 0.01 and 0.62 ± 0.01 for ceftriaxone sodium and ceftriaxone (E)-isomer respectively. The method was validated by studying Specificity, Linearity, Accuracy, Precision, Robustness, Limit of Detection (LOD) and Limit of Quantification (LOQ) and Solution stability. The developed method was successfully, sensitive, simple, precise, accurate, robust and applicable for the simultaneous determination of ceftriaxone sodium and ceftriaxone (E)-isomer in powder for injection formulation.

Rapid and Effective Determination of Ethyl Glucuronide in Hair by Micro Extraction by Packed Sorbent (MEPS) and LC-MS/MS.

Ethyl glucuronide (EtG) in hair is a reliable biomarker of alcohol consumption habits. Due to its small concentration incorporated into hair, analytical methods sensitive enough to reliably quantify EtG in this matrix are required. Sample preparation is critical in hair analysis, especially for EtG, for which extraction efficiency and matrix effect can strongly influence the results; furthermore, miniaturized methods are sought, to reduce solvent use and times of sample preparation. A micro extraction by packed sorbent (MEPS) procedure coupled to a high-performance liquid chromatography-tandem mass spectrometry method was developed and validated for quantitation of EtG in human hair samples. Fifty milligrams of hair samples were cut into snippets and extracted in water. The cleanup of the extract was carried out by using a MEPS syringe packed with anion exchange sorbent (SAX); all parameters for conditioning, washing, loading and eluting steps were optimized and the eluted aqueous volume was directly injected in the LC-MS/MS system operating in the negative ionization mode. The method was fully validated assessing LOD, LOQ, calibration curve, repeatability, accuracy, matrix effect and carryover. The method was subsequently applied to QCs and authentic hair samples. The developed MEPS method is quick and effective, with low solvent purchase and discard costs, allowing the differentiation between social drinkers and chronic excessive alcohol consumers, according to the cut-offs established by the Society of Hair Testing (SoHT).

Finite element analysis of 2.5D packaging processes based on multi-physics field coupling for predicting the reliability of IC components

The 2.5D packaging technology is a high–performance method for electronic packaging. This study addresses the reliability issues of 2.5D packaging during the manufacturing process. A multi–physics field coupling Finite Element Method (FEM) has been developed, combined with sub–modeling techniques, to investigate the curing of underfill adhesive, the curing of Epoxy Molding Compound (EMC), and the reflow soldering between the interposer and substrate in a 2.5D packaging entity during various manufacturing procedures. The focus is on the thermo–mechanical–chemical behavior of viscoelastic components within the packaging structure, as well as the viscoplastic characteristics of the micro solder balls and microbumps. A systematic analysis is conducted on the warpage deformation and stress distribution of the 2.5D packaging at crucial time points. The results demonstrate that after curing, the overall warpage of the packaging exhibits a ‘concave’ warpage profile. Additionally, as the thickness of the EMC above the chip increases, the warpage value of the packaging also increases. The warpage value defined by linear elasticity is larger than that defined by viscoelasticity. The maximum Von Mises stress value in the key areas of the submodel is greater than the maximum Von Mises stress value in the corresponding key areas of the global model. After reflow soldering, the stress concentration in the micro solder balls occurs at the edge of the micro solder ball array. The maximum stress values for each component of the packaging are observed in the interface areas between the components. Packaging components that undergo the curing process have notably higher warpage and Von Mises stress values than those that do not undergo the curing process. The simulation method established in this study can accurately predict the warpage deformation and stress distribution state of 2.5D packaging, providing significant engineering application value for process optimization and reliability enhancement of 2.5D packaging in the production process.

Stability-indicating high-performance thin-layer chromatography method development and validation for the simultaneous estimation of azithromycin, fluconazole, and secnidazole in active pharmaceutical ingredient and its tablet dosage form

Stability-indicating high-performance thin-layer chromatography method development and validation for the simultaneous estimation of azithromycin, fluconazole, and secnidazole in active pharmaceutical ingredient and its tablet dosage form

High performance method for COPD features extraction using complex network.

Objectives. The paper proposes a novel methodology for the classification of Chronic Obstructive Pulmonary Disease (COPD) utilizing respiratory sound attributes.Methods. The approach involves segmenting respiratory sounds into individual breaths and conducting extensive studies on this dataset. Spectral Transforms, various Wavelet Transforms are applied to capture distinct signal features. Complex Network is also employed to extract characteristic elements, generating novel representations of spectrogram data based on graph factors, including entropy, density, and position. The normalized and enriched data is then used to develop COPD classifiers using six machine learning algorithms, fine-tuning with appropriate training details and hyperparameter tuning.Results. Our results demonstrate robust performance, with ROC curves consistently exhibiting an Area Under the Curve (AUC) > 96% across different time-frequency transformations. Notably, the Random Forest algorithm achieves an AUC of 99.67%, outperforming other algorithms. Moreover, the Wavelet Daubechies 2 (Db2) consistently approaches 98% accuracy, particularly noteworthy in conjunction with the Naive Bayes algorithm.Conclusion. This study diagnosis patients through spectrogram images extracted from lung sounds. The application of Inverse Transforms, Complex Network, and Optimized Classification Algorithms yielded results beyond expectations. This methodology provides a promising approach for accurate COPD diagnosis, leveraging Machine Learning techniques applied to respiratory sound analysis.

Bioequivalence Analysis of Clindamycin Hydrochloride Capsules in Healthy Chinese Subjects Under Fasted and Fed Conditions.

Clindamycin is a lincosamide antibiotic for the treatment of staphylococcal, streptococcal, and anaerobic bacterial infections. We conducted a single-center, single-dose, 2-preparation, 2-period, 2-sequence, randomized, open-label, 2×2 crossover study to evaluate the pharmacokinetics (PKs) and safety of the test and reference clindamycin hydrochloride capsules in healthy Chinese subjects under both fasted and fed conditions. Forty-eight subjects were enrolled in the study totally, with 24 subjects in each group. All subjects were asked to take a test or reference preparation, under either fasted or fed condition, and their blood samples were collected and assayed by a validated high-performance liquid chromatography-tandem mass spectrometry method. PK parameters including maximum plasma concentration, area under the plasma concentration-time curve from time 0 to the last concentration, and area under the plasma concentration-time curve from time 0 to infinity were estimated with noncompartmental model and analyzed. Results showed that the PK profiles of the 2 preparations were consistent and met the bioequivalence criteria. Food was identified as a factor that had an impact on clindamycin absorption. The safety of clindamycin hydrochloride capsules was satisfactory. This study proved that the 2 clindamycin hydrochloride capsules were bioequivalent in healthy Chinese subjects under both fasted and fed conditions.

FTDZOA: An Efficient and Robust FS Method with Multi-Strategy Assistance.

Feature selection (FS) is a pivotal technique in big data analytics, aimed at mitigating redundant information within datasets and optimizing computational resource utilization. This study introduces an enhanced zebra optimization algorithm (ZOA), termed FTDZOA, for superior feature dimensionality reduction. To address the challenges of ZOA, such as susceptibility to local optimal feature subsets, limited global search capabilities, and sluggish convergence when tackling FS problems, three strategies are integrated into the original ZOA to bolster its FS performance. Firstly, a fractional order search strategy is incorporated to preserve information from the preceding generations, thereby enhancing ZOA's exploitation capabilities. Secondly, a triple mean point guidance strategy is introduced, amalgamating information from the global optimal point, a random point, and the current point to effectively augment ZOA's exploration prowess. Lastly, the exploration capacity of ZOA is further elevated through the introduction of a differential strategy, which integrates information disparities among different individuals. Subsequently, the FTDZOA-based FS method was applied to solve 23 FS problems spanning low, medium, and high dimensions. A comparative analysis with nine advanced FS methods revealed that FTDZOA achieved higher classification accuracy on over 90% of the datasets and secured a winning rate exceeding 83% in terms of execution time. These findings confirm that FTDZOA is a reliable, high-performance, practical, and robust FS method.

A New Megastigmane Nor-sesquiterpene Isolated from Pourouma Guianensis by High-Performance Countercurrent Chromatography

Introduction: Pourouma guianensis (Urticaceae) is widespread throughout Brazil and is commonly known as “mapati”. Terpenes are common in Urticaceae species. However, few studies have reported the isolation and characterisation of these compounds in Pourouma genus. Method: The aim of this study was to separate substances from stem barks of P. guianensis using a high-performance countercurrent chromatography gradient elution method. The dichloromethane extract of the P. guianensis stem bark was submitted to silica gel column chromatography, yielding three fractions. Fraction 3 was submitted to a gradient elution system in high-performance countercurrent chromatography using two solvent systems, hexane/ethyl acetate/methanol/water (1:2:x:1, x=1.0 and 1.5). Six compounds were isolated. Results: A new megastigmane nor-sesquiterpene named 2-acetyl-4,7-epoxy-3-oxy-5,5,9- trimethylhexahydrocoumaran (1) was obtained together with five known terpenes: vomifoliol (2), 2α,3β,19α,23-tetrahydroxyurs-12-en-28-oic acid (3), 3-β-D-arabinopyranoside-19-hydroxyurs-12-en- 28-oic acid (4), arjunolic acid (5), and tormentic acid (6). Fractions 1 and 2 were purified by binary gradient elution from hexane to ethyl acetate. Conclusion: This process isolated three known compounds: friedelin (7) and 3β-friedelanol (8) from fraction 1, and β-sitosterol (9) from fraction 2. Gradient elution in countercurrent chromatography was a suitable alternative, exploiting variations in the partition coefficient between substances with small structural differences.

Dual signal amplification strategy-based electrochemical aptasensor utilizing redox molecule/MOF composites for multi-pesticide detection

Electrochemical aptasensor is a great tool for simultaneously assessing harmful pesticide residues in agricultural products and foods. This study ingeniously designed an electrochemical aptasensor based on dual signal amplification strategies for concurrent detection of various pesticide residues. Firstly, poly(diallyldimethylammonium chloride)-functionalized reduced graphene oxide (PR) and Au-Pt-Pd trimetallic nanoflowers supported on HP-UiO66-NH2 were creatively employed together as substrates to load more aptamers, ascribed to the improved conductivity, abundant sites and a large electrochemical effective surface area. Secondly, ferrocene-cysteine gold nanoparticles supported on CeMOF(Ⅲ, Ⅳ) and methylene blue-loaded MOF235 were innovatively engineered to build two distinctive signal labels, which displayed comparable large and stable signal currents among other redox molecule/MOF composites. Additionally, PR contributed further signal amplification. Consequently, the constructed aptasensor showed superior performance for simultaneous detection of acetamiprid (AD) and malathion (ML), with linear ranges from 10 pM to 0.1 μM and detection limits of 4.8 pM for AD and 0.51 pM for ML. Moreover, the aptasensor performed well in the assay of AD and ML in Chinese cabbage samples with high accuracy compared with a high-performance liquid chromatography-tandem mass spectrometry method. Overall, the strategies proposed herein provided a useful and potential route for general development of electrochemical aptasensors to simultaneously detect multiple pesticide residues.

Quantitation of the DNA-dependent protein kinase inhibitor peposertib (M3814) and metabolite in human plasma by LC-MS/MS.

The DNA-dependent protein kinase (DNA-PK) is an abundant nuclear protein that mediates DNA double-strand break repair by nonhomologous end joining (NHEJ). As such, DNA-PK is critical for V(D)J recombination in lymphocytes and for survival in cells exposed to ionizing radiation and clastogens. Peposertib (M3814) is a small molecule DNA-PK inhibitor currently in preclinical and clinical development for cancer treatment. We have developed a high-performance liquid chromatography-mass spectrometry method for quantitating peposertib and its metabolite in 0.1 mL human plasma. After MTBE liquid-liquid extraction, chromatographic separation was achieved with a Phenomenex Synergi polar reverse phase (4μm, 2× 50 mm) column and a gradient of 0.1% formic acid in acetonitrile and water over an 8min run time. Mass spectrometric detection was performed on an ABI SCIEX 4000 with electrospray, positive-mode ionization. The assay was linear from 10 to 3000 ng/mL for peposertib and 1-300 ng/mL for the metabolite and proved to be both accurate (97.3%-103.7%) and precise (<8.9%CV) fulfilling criteria from the Food and Drug Administration (FDA) guidance on bioanalytical method validation. This liquid chromatography-tandem mass spectroscopy (LC-MS/MS) assay will support several ongoing clinical studies by defining peposertib pharmacokinetics.

A Polyacrylate Cotton-based Pipette Tip Micro-solid-phase Extraction Technique Coupled with High-performance Liquid Chromatography for Carvedilol Determination in Aqueous Media

Introduction: In this work, a polyacrylate polymer was synthesized into a pipette tip containing cotton fibers and used to extract carvedilol from water and urine samples. Methods: A high-performance liquid chromatography-ultraviolet detection method was developed, which demonstrated the suitability of the purposed pipette tip micro-solid-phase extraction device. Factors affecting the fabrication procedure and polymer quality were studied and optimized. In the next step, the sample preparation process (including extraction and desorption) was fully optimized, and the optimized method was validated. Results: A coating with suitable mechanical and chemical stability was achieved. Its structure was successfully characterized by Fourier transform infrared spectroscopy and scanning electron microscopy. Within-batch and between-batch fabrication reproducibility were obtained at 3.0 and 9.0 %, respectively. The developed method displayed a limit of detection of 1.1 µg L-1 when 1.5 mL of sample was processed, and it was linear in the concentration range of 3.3-350 µg L-1 with LLOQ of 5 µg L-1 . The polyacrylate cotton-based pipette tip was finally used to extract carvedilol from aqueous media with acceptable recoveries of 92-106%. Conclusion: The proposed method is simple and fast and requires low sample volumes. In addition, this method has been evaluated in terms of greenness with three different tools, and the evaluation results with all three tools have shown that this method is one of the green and environmentally friendly methods.

A validated high-performance liquid chromatography-ultraviolet method for the determination of valproic acid derivatives in pharmaceutical formulations with a microbiological suitability evaluation

Valproic acid and its derivatives are common drugs used in the treatment of epilepsy, a result of CNS disorders. Because the molecular structure of valproic acid, as a fatty acid, does not contain any chromophore groups, its peak response demanded special conditions to be detected in HPLC, ensuring the best precision results. Still, the current approach illustrates simple, validated procedures for conduction. The conducted chromatographic system consists of the BDS Hypersil C8, 150 × 4.6 mm, 5 µm column using a mobile phase of acetonitrile: phosphate buffer (4:6) at a detection wavelength of 215 nm at room temperature. A full method validation study was conducted and approved to ensure precise, repeatable, and accurate results by implementing system suitability parameters. In microbiological terms, a suitability test is used to validate microbiological testing methods, ensuring their efficacy despite potential interference from antimicrobial properties in the tested materials. The HPLC-UV developed and validated analytical method was evaluated, and it was found to be sensitive for use in the detection of low concentrations of methylparaben, propylparaben, and valproate with an optimum run time of six minutes. limit of detection (LODs) were statistically estimated and found to be 2.27 µg/mL, 39.77 ng/mL, and 1.84 µg/mL for methylparaben, propylparaben, and valproate, respectively. Additionally, the method demonstrated a high recovery of methylparaben, propylparaben, and valproate with an excellent closed-accuracy range (98.84% - 101.34%). An excellent regression coefficient (r) of 0.99924, 0.99998, and 0.99997 for methylparaben, valproate, and propylparaben, respectively, was achieved. Assay determination of various pharmaceutical dosage forms in the local market was implemented, yielding admirable results.

Validation and optimisation of reduced glutathione quantification in erythrocytes by means of a coulometric high-performance liquid chromatography analytical method.

Glutathione (GSH), a tripeptide that consists of cysteine, glutamate and glycine, is present in all mammalian tissues in the millimolar range. Besides having numerous cellular functions, GSH is an important antioxidant and is considered a valuable biomarker in evaluating oxidative stress. This paper provides a sensitive analytical method using HPLC-ECD to quantify GSH in erythrocytes, validated using the ICH guidelines for Bioanalytical Method Validation. The sample preparation was optimised using centrifugal filtration and a hypotonic phosphate buffer for extracting GSH from erythrocytes. HPLC-ECD parameters were adjusted to allow a fast, reversed phase, isocratic separation in 10min. The detector response was linear between 0.3 and 9.5μg/mL with a satisfactory regression coefficient and a LOQ of 0.11 μg/mL. Intra- and inter-day repeatability ranged between 1.10% and 8.57% with recoveries ranging from 94.3% to 106.0%. Dilution integrity, benchtop, freeze-thaw and long-term stability were investigated. Samples were stable for up to 6months at -80°C. This method has a good linear response and is repeatable, precise and accurate. It minimises GSH auto-oxidation using a centrifugal filter during sample preparation, instead of acidification. Therefore, this analytical method is suitable for quantifying GSH in erythrocytes as a marker of oxidative stress.

Design of different oxygen content and high performance bilayer In2O3 thin-film transistors at room temperature for flexible electronics

In this study, homojunction bilayer In2O3thin film transistors (TFTs) were prepared by RF-magnetron sputtering at room temperature. Herein, an active channel of bilayer In2O3TFTs are consist of the front channel with lower (poor) oxygen content and the back channel with higher (rich) oxygen content. Therefore, optimizedbilayer In2O3TFT was fabricatedandaμFE of 32.5 cm2/Vs and a small SS of 280 mV/decade, a small VTH of 0.3 Vwere achieved. In addition, small VTH shifts of 0.7 (−1.0) and 0.4 (−1.2) V under gate bias and light illumination stress tests were obtained. Through XPS band structure analysis indicated that the formation of band bending between the channel layers leads to electron injection from the back channel into the front channel, resulting in accumulation of forming carriers near the interface of the bilayer, resulting in increase the μFE of In2O3TFTs. Furthermore, XPS and LFN measurement demonstrate that control the oxygen content can reduced the oxygen-related defects and bulk/interface trap density while controlling the Ne and carrier transport in the bilayer In2O3 film,which enhance the stability of In2O3TFTs. Overall, the high-performance bilayer In2O3TFTshave opena new method to obtaine the flexible electronic devices.

Development of Amla Nutri-bar: Proximate analysis, gallic acid quantification and its validation through HPTLC, and spectroscopy

BACKGROUND: “Ayush Ahara” confluences advanced food technology with Ayurveda to develop dietary products rooted in traditional medicine. Here, Amla (Indian gooseberry), a medicinal fruit well-known for its health benefits, was used to develop a novel dietary product—Amla Nutri-bar (ANB). Furthermore, this research aims to substantiate its therapeutic potential through quality control analysis. METHODS: Three batches of ANB were prepared at the pharmaceutical laboratory, All India Institute of Ayurveda, New Delhi, India. These were evaluated for sensory attributes using a 9-point hedonic scale and underwent physicochemical, phytochemical, total phenolic content, chromatographic, and spectroscopy assays. RESULTS: The sensory evaluation indicated positive feedback, with an overall acceptability score of 8, followed by taste and flavor rated at 7 Physiochemical constants included pH: 2.2, moisture: 11.48%w/w, total ash: 0.17%w/w, water-soluble extractive value: 88.4%w/w, and alcohol-soluble extractive value: 56.65%w/w. Phytochemical screening revealed that the product is rich in flavonoids, tannins, and alkaloids. Nutritional composition per 100 g had energy: 373.76 kcal, proteins: 1.61%, carbohydrates: 88.59% by wt, dietary fiber: 2.72 g, total fat: 1.44%, vitamin C: 300.11 mg, vitamin A: 71.23 pg, iron: 5.63 mg, calcium: 126.69 mg, and potassium: 103.57 mg. Total phenolic content was 4.95 mg gallic acid equivalents/g, with gallic acid quantified at 270.4 μg/100 mg employing a validated high-performance thin layer chromatography method. Fourier transform infrared spectroscopy analysis showed the presence of alcohol, phenol, and alkanes. All the tested pesticide residues were found below detection limits. CONCLUSION: ANB can be a food product that is, not delicious only but can also contribute significantly to overall health and well-being.

High-Performance Liquid Chromatography-Tandem Mass Spectrometry Method Development and Validation for Simultaneous Determination of Seven Nitrosamine and Azidomethyl-Biphenyl-Tetrazole Impurities in Losartan.

Nitrosamine-related impurities (N-nitrosomethylamino butyric acid [NMBA], N-nitrosodiethylamine [NDEA], N-nitrosodiisopropylamine [NDIPA], N-nitrosomethylphenylamine [NMPA], N-nitrosodibutylamine [NDBA], N-nitrosodimethylamine [NDMA], and N-nitrosoethylisopropylamine [NEIPA]) and 5-[4'-(azidomethyl)-[1,1'-biphenyl]-2-yl]-2H-tetrazole (AZBT) formed during the manufacture of sartan medicines have been classified into human mutagens and carcinogens after long-term treatment. The study developed a simple, economical but highly sensitive procedure for the simultaneous quantification of seven nitrosamines and AZBT impurities in sartan pharmaceuticals. After extraction with methanol (MeOH) 50%, the compounds were analyzed with a reversed-phase liquid chromatography-tandem mass spectroscopy with atmospheric-pressure chemical ionization (APCI) mode (APCI[+] for nitrosamines and APCI[-] for AZBT), selected reaction monitoring, C18 column, gradient elution with 0.1% formic acid in water and in MeOH, respectively. The validated procedure obtained high extraction efficiency (>90%), wide linear range (0.2-50.0ng/mL NMBA, NDEA, NDIPA, NMPA, and NDBA; 0.5-50.0ng/mL NDMA and NEIPA; 2.0-100ng/mL AZBT), limit of quantification <10% of the acceptance level, recovery range of 85%-115% with relative standard deviation <15% and minimum matrix effects for all impurities. The procedure was applied to test 16 commercial losartan samples. As a result, eight samples contained AZBT within the current regulatory limits, but no nitrosamine impurities were detected in all samples.

High-Performance Grape Disease Detection Method Using Multimodal Data and Parallel Activation Functions

This paper introduces a novel deep learning model for grape disease detection that integrates multimodal data and parallel heterogeneous activation functions, significantly enhancing detection accuracy and robustness. Through experiments, the model demonstrated excellent performance in grape disease detection, achieving an accuracy of 91%, a precision of 93%, a recall of 90%, a mean average precision (mAP) of 91%, and 56 frames per second (FPS), outperforming traditional deep learning models such as YOLOv3, YOLOv5, DEtection TRansformer (DETR), TinySegformer, and Tranvolution-GAN. To meet the demands of rapid on-site detection, this study also developed a lightweight model for mobile devices, successfully deployed on the iPhone 15. Techniques such as structural pruning, quantization, and depthwise separable convolution were used to significantly reduce the model’s computational complexity and resource consumption, ensuring efficient operation and real-time performance. These achievements not only advance the development of smart agricultural technologies but also provide new technical solutions and practical tools for disease detection.

Development and Validation of a High-Performance Thin-Layer Chromatography Method for the Qualitative Analysis and Quantification of Hispidulin in Hydroethanol Extract of S. barbata D. Don

Background: Hispidulin, a flavonoid renowned for its diverse pharmacological activities, is abundant in S. barbata D. Don. Given its prevalence, it is essential to establish a dependable analytical method for quantifying hispidulin in this plant. Methods: This study introduces a sensitive and reliable high-performance thin-layer chromatographic (HPTLC) method for both qualitative and quantitative analysis of hispidulin in S. barbata D. Don. Pre-coated TLC aluminum plates were utilized, and after testing various mobile phase combinations, the most effective separation was achieved with Toluene-ethyl acetate-formic acid (5:4:1, v/v/v). The method underwent extensive validation for linearity, specification, instrument precision, precision, limits of LOD and LOQ, accuracy, and robustness. Results: The developed method demonstrated excellent linearity over a specified concentration range, with a determination coefficient (r2) of 0.988. A well-defined spot at Rf 0.7, corresponding to hispidulin, was observed. The concentration of hispidulin in the hydroethanolic extract of S. barbata D. Don was quantified as 13.02 μg/mg of extract. Conclusion: In conclusion, the HPTLC method presented in this study offers a simple, accurate, and robust tool for quantitatively analyzing hispidulin in the hydroethanol extract of S. barbata D. Don. This method is suitable for routine quality control and standardization of herbal formulations containing S. barbata D. Don, thereby contributing to the advancement of research in natural product- based pharmaceuticals.

Development and validation of High-Performance Thin Layer Chromatographic methods for simultaneous determination of antibacterial pharmaceutical formulations containing Clindamycin phosphate.

The main objective of this research is to establish and authenticate the High-Performance Thin-Layer Chromatographic techniques for the simultaneous assessment of Clindamycin phosphate in combination with Tretinoin (formulation-1) and Clindamycin phosphate with Adapalene (formulation-2), both of which are antimicrobial combinations. In the developed HPTLC methods, for combination-1, the optimized mobile phase was a mixture of n-Hexane: Ethyl acetate: ACN: Methanol (5:2:2:1 by volume) with observed Rf values of 0.413 and 0.787 for Clindamycin phosphate and Tretinoin, respectively. Similarly, for combination-2, the mobile phase comprised n-Hexane: Diethyl ether: Dichloromethane: Acetic acid (4:4:2:0.1 by volume) with recorded Rf values of 0.407 and 0.559 for Clindamycin phosphate and Adapalene, respectively. The developed methods are successfully validated as per the regulatory guidelines. This approach proves to be significantly time-saving and costeffective, rendering it suitable for routine analyses of the formulations containing selected antibacterial active pharmaceutical ingredients and commercial formulations.

Stability-indicating high-performance thin-layer chromatography method development and validation for dapagliflozin propanediol monohydrate, vildagliptin, and metformin hydrochloride in active pharmaceutical ingredient and its tablet dosage form

Stability-indicating high-performance thin-layer chromatography method development and validation for dapagliflozin propanediol monohydrate, vildagliptin, and metformin hydrochloride in active pharmaceutical ingredient and its tablet dosage form