Rapid, Simple and Low-Cost Analytical Method Development for Quantification of Eltrombopag Olamine in Tablet Dosage by UV Spectroscopy Method.

BACKGROUND: Eltrombopag Olamine is a drug used to treat thrombocytopenia, a disorder where blood platelet counts get lower and severe aplastic anemia. It serves as a thrombopoietin receptor agonist, which give rise to platelet production in the bone marrow. OBJECTIVES: The objective of this study is to develop a simple, specific, accurate, precise and economical Ultraviolet spectroscopy method to estimate the amount of Eltrombopag Olamine in bulk and tablet dosage form. METHODS: The developed method was performed using methanol for identification and physicochemical characterization of the drug. The validation parameters like linearity, precision, accuracy, robustness limits of detection and quantitation, and specificity were assessed as per ICH Q2 (R2). RESULTS: The maximum absorbance wavelength (λmax) of the drug was found at 247 nm in methanol. The linearity was found in the concentration range of 2-14 µg/ml with regression equation y = 0.0619x - 0.0123 and r² = 0.999. The standard addition method was used to determine the accuracy of the developed method. The result was found in the % recovery range of 98-99%. The precision was done on λmax with respect to the parameters such as repeatability, intraday, and interday. The method was found to be precise as the % RSD value was found to be <2%. The detection limit value (LOD) and quantitation limit value (LOQ) were 0.0524 µg/ml and 0.1588 µg/ml, respectively. CONCLUSION: The developed method is simple, economical, accurate and selective. The developed method was adaptable for the estimation of Eltrombopag Olamine analysis in pharmaceutical dosage form and routine quality control laboratory.

Titanium dioxide in face powders and eyeshadows: Developing an analytical methodology for accessing customer safety.

BACKGROUND: Titanium dioxide (TiO2), a white powder, represents the opacifier used in many products, including drugs, foods, cosmetics, paints, and dyes. METHOD: The Uv-Vis spectrophotometry was a particularly suitable technique to quantify TiO2 in the solutions obtained from cosmetics. In this work, we determined the TiO2 content in a total of 88 samples of eye shadows and face powders of different brands and costs. Before to analyse the samples, we developed the mineralization and analysis method, in fact, fusion with potassium bisulphate would be very laborious because it must be carried out on one sample at a time and requires very long times, instead, the mineralization with the acid mixture and the aid of microwaves allowed us to solubilize six samples at the same time within 45 min. RESULTS: From the results obtained, we can state that the highest concentrations of TiO2 are found in the eyeshadows with a maximum value of 36% in a blue eyeshadow.

Matrix-matched quantification of volatile organic compounds (VOCs) in gluten free flours and bakery products.

The aim of this study deals with characterize the volatile profiles of gluten free flours and bakery products. An appropriate HS-SPME/GC-MS methods for the quantification analyses was performed and corn starch solid as standards was used. 34 different samples were analysed, and 127 compounds distributed in 4 classes (alcohols, aldehydes and ketones, heterocyclic compounds, and terpenes), that make up the aroma of these gluten free, were identified. The developed method is characterized by detection limits of 0.0004 and 0.0047 mg/kg for camphor and pyrazine, respectively, and linearity of quantification standards were between 0.990 and 0.998 for a range of 3-50 mg/kg.

The carcinogenic PAHs in breads, amount, analytical method and mitigation strategy, a systematic review study.

Bread is one of the most consumed foods all over the world. Several contaminants are identified in bread. Polycyclic aromatic hydrocarbons (PAHs) is one of these contaminants. This systematic study evaluates the amount of four carcinogenic PAHs (PAH4) in various types of breads. To conduct this study, a comprehensive search was carried out using keywords of polycyclic aromatic hydrocarbons, PAHs, PAH4, and bread, with no time limitations. 17 articles were selected and fully evaluated. The observed range of PAH4 concentrations in bread varied from non-detected (ND) to 20.66 µg/kg. In the sample preparation process for analysis, an ultrasonic bath was predominantly utilized. Most chromatographic methods are able to measure PAHs in food, but the GC-MS method has been used more. To mitigate PAH levels in bread, it is suggested to incorporate antioxidants during the bread-making process. Furthermore, the type of bread, the type of fuel used to bake the bread, the temperature and the cooking time were some of the factors affecting the amount of PAH. Restricting these factors could significantly reduce PAH content. Regarding the risk assessment conducted in the manuscript, it was determined that industrial breads are usually considered safe. However, some traditional breads may pose risks in terms of their potential PAH content.

Resolution-enhanced Kendrick mass defect analysis for improved mass spectrometry characterization of lignin.

Lignin is a promising renewable source of valuable organic compounds and environmentally benign materials. However, its involvement in economic circulation and the creation of new biorefining technologies require an understanding of its chemical composition and structure. This problem can be overcome by applying mass spectrometry analytical techniques in combination with advanced chemometric methods for mass spectra processing. The present study is aimed at the development of mass defect filtering to characterize the chemical composition of lignin at the molecular level. This study introduces a novel approach involving resolution-enhanced Kendrick mass defect (REKMD) analysis for the processing of atmospheric pressure photoionization Orbitrap mass spectra of lignin. The set of priority Kendrick fractional base units was predefined in model experiments and provided a substantially expanding available mass defect range for the informative visualization of lignin mass spectra. The developed REKMD analysis strategy allowed to obtain the most complete data on all the homologous series typical of lignin and thus facilitated the interpretation and assignment of elemental compositions and structural formulas to oligomers detected in extremely complex mass spectra, including tandem ones. For the first time, the minor modifications (sulfation) of lignin obtained in ionic liquid-based biorefining processes were revealed.

Set up and validation of a method to analyse microplastics in stool and small intestine samples.

The contamination of microplastics in humans is of increasing concern. Therefore, the aim of this study was to develop effective methods to determine the concentration and types of microplastics entering human digestive system. To study levels of MPs contamination in humans, an excellent indicator are stools. Indeed, stools, and thus the digestive system, can be an excellent indicator of the level of MPs contamination in humans. Hence, objective was to find effective methods to extract, quantify and characterize microplastics in stool and small intestine samples. The samples studied were human stools and pig jejunum (which has human-like characteristics). The methods were optimized by observing extraction efficiency, compatibility by Fourier-transform infrared spectroscopy (FTIR) characterization and non-deformation of the microplastics. The steps of the procedure were: • Sampling to avoid plastic contamination • Non-aggressive chemical and enzymatic digestion • Counting and characterization The methods were optimized and validated, observing recovery and repeatability. Therefore, two simple, effective methods with high analytical performance have been developed. The MPs present in the stool and intestine samples were counted by stereoscopic microscope and characterized by FTIR, finding several types of MPs such as synthetic cellulose, polyethylene, polypropylene, polystyrene, and polyethylene terephthalate, among others.

Simultaneous Estimation of Quercetine and Betanine by RP-HPLC from Herbal Formulations Used in Nutritional Deficiencies.

BACKGROUND: Medicinal plants have curative properties due to the presence of various complex chemical substances of different compositions, which are found as secondary plant metabolites in one or more parts of the plants. Moringa oleifera from Moringaceae and Beta vulgaris root are, native to India, grows in the tropical and subtropical regions of the world. It is commonly known as 'drumstick tree' or 'horseradish tree' or 'miracle tree'. Incorporation of more herbal powder leads to much complexity. Above plants were chosen for their utmost nutritional values. RESULTS: Herbal tablet and granules were prepared and evaluated further for various Physico-chemical parameters as a nutritional supplement. Promising results indicate that prepared formulations have potential as supplements. CONCLUSIONS: Present communication mainly focused on estimation of marker components by Reverse Phase-High Performance Liquid Chromatography. It showed the presence of enough number of secondary metabolites and minerals which can be easily consumed by all age groups.

Application of newly developed and validated LC-MS/MS method for pharmacokinetic study of adagrasib and pembrolizumab simultaneously in rat plasma.

Non-small cell lung cancer (NSCLC) is a significant subtype of lung cancer, and poses a dangerous global threat. One of the current approaches of NSCLC treatment is a combination therapy of adagrasib and pembrolizumab. Accurate monitoring of these drug concentrations in biological fluids is critical for treatment efficacy. Since no method was reported for simultaneous estimation of these drugs, this study focuses on the development of a validated LC-MS/MS bioanalytical method for simultaneous quantification of Adagrasib and Pembrolizumab in rat plasma. The analytes were extracted from the biological matrix through liquid-liquid extraction techniques using acetonitrile as extraction solvent. The analytes were separated on a Waters X-bridge phenyl C18 column, with a mixture of acetonitrile: 0.1 % TFA in water (50: 50 v/v) as mobile phase at an isocratic flow rate of 1.0 mL/min with a runtime of about 5 min. Adagrasib (m/z 605.12 → 201.62), Pembrolizumab (m/z 146.32 → 85.15), and Sotorasib (m/z 561.59 → 218.92) were determined by recording the mass spectra through multiple reaction monitoring in positive mode. The method was validated according to USFDA guidelines. The results demonstrate satisfactory linearity with an r2 value of 0.9998 in the ranges of 40-800 and 10-200 ng/mL, accuracy with mean percentage recovery of 95.22-98.59 % and 96.98-98.57 %, precision indicated with %RSD ranged between 0.39-1.91 % and 0.85-9.03 % for Adagrasib and Pembrolizumab respectively, and other key parameters. The developed method can determine the pharmacokinetic parameters to indicate the efficacy and safety of the drugs, and also can quantify selected drugs simultaneously in biological samples.

Food adulteration: Causes, risks, and detection techniques-review.

Food adulteration is the intentional addition of foreign or inferior substances to original food products for a variety of reasons. It takes place in a variety of forms, like mixing, substitution, hiding poor quality in packaging material, putting decomposed food for sale, misbranding or giving false labels, and adding toxicants. Several analytical methods (such as chromatography, spectroscopy, electronic sensors) are used to detect the quality of foodstuffs. This review provides concise but detailed information to understand the scope and scale of food adulteration as a way to further detect, combat, and prevent future adulterations. The objective of this review was to provide a comprehensive overview of the causes, risks, and detection techniques associated with food adulteration. It also aimed to highlight the potential health risks posed by consuming adulterated food products and the importance of detecting and preventing such practices. During the review, books, regulatory guidelines, articles, and reports on food adulteration were analyzed critically. Furthermore, the review assessed key findings to present a well-rounded analysis of the challenges and opportunities associated with combating food adulteration. This review included different causes and health impacts of food adulteration. The analytical techniques for food adulteration detection have also been documented in brief. In addition, the review emphasized the urgency of addressing food adulteration through a combination of regulatory measures, technological advancements, and consumer awareness. In conclusion, food adulteration causes many diseases such as cancer, liver disease, cardiovascular disease, kidney disease, and nervous system-related diseases. So, ensuring food safety is the backbone of health and customer satisfaction. Strengthening regulations, taking legal enforcement action, enhancing testing, and quality control can prevent and mitigate the adulteration of food products. Moreover, proper law enforcement and regular inspection of food quality can bring about drastic changes.

PicoGreen assay for nucleic acid quantification - Applications, challenges, and solutions.

Various analytical methods and reagents have been employed for nucleic acid analysis in cells, biological fluids, and formulations. Standard techniques like gel electrophoresis and qRT-PCR are widely used for qualitative and quantitative nucleic acid analysis. However, these methods can be time-consuming and labor-intensive, with limitations such as inapplicability to small RNA at low concentrations and high costs associated with qRT-PCR reagents and instruments. As an alternative, PicoGreen (PG) has emerged as a valuable method for the quantitative analysis of nucleic acids. PG, a fluorescent dye, enables the quantitation of double-stranded DNA (dsDNA) or double-stranded RNA, including miRNA mimic and siRNA, in solution. It is also applicable to DNA and RNA analysis within cells using techniques like FACS and fluorescence microscopy. Despite its advantages, PG's fluorescence intensity is affected by various experimental conditions, such as pH, salts, and chemical reagents. This review explores the recent applications of PG as a rapid, cost-effective, robust, and accurate assay tool for nucleic acid quantification. We also address the limitations of PG and discuss approaches to overcome these challenges, recognizing the expanding range of its applications.

Update on chromium speciation analysis in foods: a review of advances in analytical methods and dietary exposure assessment.

Chromium occurs naturally in different oxidation states. Amongst them, hexavalent chromium is classified as both genotoxic and carcinogenic while trivalent chromium can be considered as an essential element. Therefore, speciation analysis is essential when conducting dietary exposure assessment. Several critical reviews have been published on chromium speciation analysis in foodstuffs in the last decade. However, a method that can account for species interconversion during the extraction procedure has not been reported in the reviews. In recent years, an online method using species-specific isotope dilution mass spectrometry has been developed for the simultaneous determination of trivalent and hexavalent chromium in foodstuffs. Apart from that, new methods based on offline analytical techniques, to analyse trivalent and hexavalent chromium separately, are still under development. Therefore, one of the objectives of this paper is to review these recently published analytical methods and assess whether they are fit for chromium speciation analysis in foodstuffs. Additionally, an objective is also to assess whether their limits of detection are sufficiently low for dietary exposure assessment with respect to the neoplastic effects of hexavalent chromium. Moreover, possible future research gaps are identified based on the current knowledge and existing literature.

Ultraviolet spectrophotometry as method to determine the concentration of ß-myrcene released from chitosan in aqueous medium.

Myrcene (ß-myrcene), found in essential oils from plant species such as hops and cannabis, has many advantageous properties, but its use is limited due to volatility and low solubility in water. One way to circumvent these limitations is to encapsulate the essential oils in a polymer matrix. However, these hydrophobic molecules are difficult to quantify when dispersed in water. Seeking to study the release of this terpene in drug release tests from polymeric matrices, this work aimed to develop an easy and cheap UV spectrophotometric method for the quantification of ß-myrcene in aqueous medium. To achieves this goal, samples were prepared in 0.05% (w/v) polysorbate 80 solution, with concentrations of ß-myrcene ranging from 0.01% to 0.1% (v/v), and were analyzed at 226 nm. Each sample was analyzed in triplicate and repeated on three different days, to evaluate the repeatability of the results. The results were subjected to Q, F and Student's t-tests. The regression parameters obtained for ß-myrcene were above 0.99 and through statistical analysis, it was possible to confirm the repeatability for the results. The values of the limits of detection and quantification indicated that the method is not affected by intrinsic factors of the equipment. The results of accuracy, robustness and selectivity showed recovery rates within acceptable limits. This demonstrates that the quantification of ß-myrcene in aqueous medium by UV spectrophotometry is feasible.

Stress analysis under centrifugal load of the multiple corrugated diaphragm coupling based on rotating shell thin film model.

Centrifugal force is one of the factors that cannot be ignored in high-speed shaft systems. The multiple corrugated diaphragm (MCD) Coupling is suitable for high-power and high-speed situations; hence, it is crucial to investigate the stress and deformation of the wave disc under centrifugal load. This paper first uses the rotating shell thin film model to derive the circumferential stress and deformation displacement of the MCD under centrifugal load. Then, the finite element method is used to verify the results obtained from the analytical solution. The results show the feasibility of using the rotating shell thin film model for centrifugal load analysis of the MCD, providing a new approach for the theoretical analysis of the MCD.

A Comprehensive Examination of UV-VIS Spectrophotometric Methods in Pharmaceutical Analysis Between 2015-2023.

BACKGROUND: Quality control is a system of validated procedures in which many samples, including active pharmaceutical ingredients and final products, are analyzed using standard or validated analytical methods. METHOD: Analytical methods used in analyzing active pharmaceutical ingredients or final products in the pharmaceutical industry can be methods registered in pharmacopeias and developed by the company itself. For this reason, published papers related to pharmaceutical analysis attract analysts and researchers' attention. In this study, pharmaceutical analysis and bioanalysis studies carried out between 2015 and 2023 were examined using Google Scholar, and the recent trends were determined for pharmaceutical analysis. Among the published papers performing conventional analytical techniques for pharmaceutical analysis, those applying UV-VIS spectrophotometry method were selected to predict a future perspective in this study. In addition to the data obtained, the current situation of the pharmaceutical industry was considered to correlate with the obtained data for pharmaceutical analysis. RESULTS: The results were presented with comparative tables and summarizing graphs. Interpreting the results allowed us to determine the trends that pharmaceutical analysis studies will lead in the future. This study can be helpful for researchers working on pharmaceutical analysis in both the industry and academia to predict future trends in pharmaceutical analysis. As a result of the literature research covering the dates 2015-2023, 56% of UV-VIS Spectrophotometric methods are used on pharmaceutical dosage forms, 27% are bulk, 16% are pure, 2% are biological materials, and 0.4% are herbal. Made from materials. Of these studies, 28% were conducted in the 200-240 nm range, 27% were conducted in the 240-300 nm range, and only 44% were conducted at >300 nm. Interpreting the results allowed us to determine the trends that pharmaceutical analysis studies will lead in the future. CONCLUSION: This study can be helpful for researchers working on pharmaceutical analysis in both the industry and academy side to predict future trends for pharmaceutical analysis.

Cyclodextrin-based ternary supramolecular deep eutectic solvents for efficient extraction and analysis of trace quinolones and sulfonamides in wastewater by adjusting pH.

BACKGROUND: Antibiotics residues can accelerate the growth of drug-resistant bacteria and harm the ecological environment. Under the effect of enrichment and biomagnification, the emergence of drug-resistant pathogenic bacteria may eventually lead to humans being ineffective to drugs in the face of bacterial or fungal disease infections in the future. It is urgent to develop an efficient separation medium and analytical method for simultaneous extraction and determination of antibiotics in the water environment. RESULTS: This work doped 2,6-Di-O-methyl-ß-cyclodextrin, randomly methyl-ß-cyclodextrin, 2-hydroxypropyl-ß-cyclodextrin with thymol:fatty acid respectively to construct non-covalent interaction-dominated pH-responsive ternary supramolecular deep eutectic solvents (SUPRADESs), which can undergo a hydrophilic/hydrophobic transition with aqueous phase to achieve an efficient microextraction. Semi-empirical method illustrated that SUPRADESs have a wide range of hydrogen bond receptor sites. We developed a SUPRADES-based analytical method combined with liquid chromatography-triple quadrupole mass spectrometry for the extraction and determination of trace quinolones and sulfonamides in wastewater. The overall limits of detection of the method were 0.0021-0.0334 ng mL-1 and the limits of quantification were 0.0073-0.1114 ng mL-1. The linearity maintained good in the spiked level of 0.01-100 ng mL-1 (R2 > 0.99). The overall enrichment factors of the method were 157-201 with lower standard deviations (≤8.7). SIGNIFICANCE: The method gave an extraction recovery of 70.1-115.3 % for 28 antibiotics in livestock farming wastewater samples from Zhejiang, China, at trace levels (minimum 0.5 ng mL-1). The results demonstrated that inducing the phase transition between SUPRADES and aqueous phase by adjusting pH for extraction is a novel and efficient pretreatment strategy. To our knowledge, this is the first application of cyclodextrin-based ternary SUPRADESs with pH-responsive reversible hydrophobicity-hydrophilicity transition behavior in wastewater analysis.

Protocol improvement and multisite validation of a digital soft agar colony formation assay for tumorigenic transformed cells intermingled in cell therapy products.

BACKGROUND AIMS: The administration of human cell-processed therapeutic products (hCTPs) is associated with a risk of tumorigenesis due to the transformed cellular contaminants. To mitigate this risk, these impurities should be detected using sensitive and validated assays. The digital soft agar colony formation (D-SAC) assay is an ultrasensitive in vitro test for detecting tumorigenic transformed cells in hCTPs. METHODS: In this study, we first evaluated the colony formation efficiency (CFE) precision of tumorigenic reference cells in positive control samples according to a previously reported D-SAC assay protocol (Protocol I) from multiple laboratories. However, the CFE varied widely among laboratories. Thus, we improved and optimized the test protocol as Protocol II to reduce variability in the CFE of tumorigenic reference cells. Subsequently, the improved protocol was validated at multiple sites. Human mesenchymal stromal cells (hMSCs) were used as model cells, and positive control samples were prepared by spiking them with HeLa cells. RESULTS: Based on the previously reported protocol, the CFE was estimated using an ultra-low concentration (0.0001%) of positive control samples in multiple plates. Next, we improved the protocol to reduce the CFE variability. Based on the CFE results, we estimated the sample size as the number of wells (Protocol II) and assessed the detectability of 0.0001% HeLa cells in hMSCs to validate the protocol at multiple sites. Using Protocol I yielded low CFEs (mean: 30%) and high variability between laboratories (reproducibility coefficient of variance [CV]: 72%). In contrast, Protocol II, which incorporated a relatively high concentration (0.002%) of HeLa cells in the positive control samples, resulted in higher CFE values (mean: 63%) and lower variability (reproducibility CV: 18%). Moreover, the sample sizes for testing were estimated as the number of wells per laboratory (314-570 wells) based on the laboratory-specific CFE (42-76%). Under these conditions, all laboratories achieved a detection limit of 0.0001% HeLa cells in hMSCs in a predetermined number of wells. Moreover, colony formation was not observed in the wells seeded with hMSCs alone. CONCLUSIONS: The D-SAC assay is a highly sensitive and robust test for detecting malignant cells as impurities in hCTPs. In addition, optimal assay conditions were established to test tumorigenic impurities in hCTPs with high sensitivity and an arbitrary false negative rate.

Development of a robust cell-based potency assay for a coxsackievirus A21 oncolytic virotherapy.

Oncolytic viruses (OV) are part of a burgeoning field of investigational oncolytic therapy (OT), in which lytic viruses dissolve advanced tumors productively and specifically. One such OT is a Coxsackievirus A21 (CVA21) based OV that is currently under clinical evaluation. A tissue culture infectious dose (TCID50) assay was used for CVA21 potency release and stability testing in early clinical development. The titer measured in this method was an extrapolated value from cytopathic effect (CPE) observed during the serial dilution but doesn't represent direct viral killing of cells. Moreover, the assay was not deemed to be optimal to carry into late phase clinical development due to limitations in assay precision, turn-around time, and sample throughput. To address these points, we developed a plaque assay to measure viral plaque forming units to measure the potency value for drug substance (DS), drug product (DP) and virus seed (master and working) stocks. In this manuscript, we describe the steps taken to develop this plaque assay for the late-stage clinical development, which include the assay qualification, validation, and robustness protocols, and describe statistical methods for data analysis. Moreover, the method was validated for linearity, accuracy, precision, and specificity. Furthermore, the plaque assay quantifies OV infectivity with better precision (32% vs 58%), with higher sample throughput (22 samples/week vs 3 samples/week) and shorter assay turnaround time (4 days vs 7 days) than the TCID50 method. This assay development strategy can provide guidance for the development of robust cell-based potency methods for OVs and other infectious viral products.

Relative Entropy Application to Study the Elastoplastic Behavior of S235JR Structural Steel.

The main issue in this work is to study the limit functions necessary for the reliability assessment of structural steel with the use of the relative entropy apparatus. This will be done using a few different mathematical theories relevant to this relative entropy, namely those proposed by Bhattacharyya, Kullback-Leibler, Jeffreys, and Hellinger. Probabilistic analysis in the presence of uncertainty in material characteristics will be delivered using three different numerical strategies-Monte Carlo simulation, the stochastic perturbation method, as well as the semi-analytical approach. All of these methods are based on the weighted least squares method approximations of the structural response functions versus the given uncertainty source, and they allow efficient determination of the first two probabilistic moments of the structural responses including stresses, displacements, and strains. The entire computational implementation will be delivered using the finite element method system ABAQUS and computer algebra program MAPLE, where relative entropies, as well as polynomial response functions, will be determined. This study demonstrates that the relative entropies may be efficiently used in reliability assessment close to the widely engaged first-order reliability method (FORM). The relative entropy concept enables us to study the probabilistic distance of any two distributions, so that structural resistance and extreme effort in elastoplastic behavior need not be restricted to Gaussian distributions.

Quantification of Etoricoxib in Low Plasma Volume by UPLC-PDA and Application to Preclinical Pharmacokinetic Study.

An ultra-performance liquid chromatography with photodiode array (UPLC-PDA) UV detection method was developed here for the first time for simple, rapid, selective and sensitive quantification of the commonly prescribed selective cyclooxygenase-2 (COX-2) inhibitor etoricoxib in low plasma volumes (50 µL). The method includes protein precipitation followed by liquid-liquid extraction, evaporation and reconstitution. A gradient mobile phase of 75:25 going to 55:45 (v/v) water:acetonitrile (1 mL/min flow rate) was applied. Total run time was 8 min, representing a significant improvement relative to previous reports. Excellent linearity (r2 = 1) was obtained over a wide (0.1-12 µg/mL) etoricoxib concentration range. Short retention times for etoricoxib (4.9 min) and the internal standard trazodone (6.4 min), as well as high stability, recovery, accuracy, precision and reproducibility, and low etoricoxib LOD (20 ng/mL) and LOQ (100 ng/mL), were achieved. Finally, the method was successfully applied to a pharmacokinetic study (single 20 mg/kg orally administered etoricoxib mini-capsule) in rats. In conclusion, the advantages demonstrated in this work make this analytical method both time- and cost-efficient for drug monitoring in pre-clinical/clinical settings.

Stability indicating high performance thin layer chromatography method development and validation for quantitative determination of tetracycline hydrochloride in tetracycline hydrochloride active pharmaceutical ingredient (API) and its dosage forms.

Simple, quick, cost-effective, and environmentally friendly analytical methods for quality assurance and control roles for different medicines, including Tetrcyclines, are most significantly needed. Also, different thin layer chromatography (TLC)-based methods for tetracycline identification exist, but high performance thin layer chromatography methods based on modern state- of- the art equipment are still nonexistent. Thus, in this study, analytical method development and verification were done by high performance thin layer chromatography (HPTLC) (using an automated equipment model) using glass plates coated with silica gel 60 F254 after treating with 10% Na2EDTA. Validation was carried out according to International Council for Harmonization (ICH) guidelines. A mobile phase formed from ethyl acetate, acetonitrile, methanol, and 1% aqueous ammonia in the composition of 4.4:19.6:10:6 volume to volume ratio (V/V) was used. Rf value, percentage recoveries, linearity ranges, limit of detection (LOD), and limit of quantitation (LOQ) for the developed HPTLC method were 0.28, 100.83-106.25%, 160-560 ng/band (r2 values of 0.9999), 31.9 ng/band, and 96.7 ng/band, respectively. The results of the sample assays conducted using the new method and the United States Pharmacopoeia (USP) high performance liquid chromatography (HPLC) method were 91.59% to 108.3% and 90.83% to 102.85%, respectively. The F test for the aforementioned methods was 2.01, which is smaller than the tabulated F value of 5.05 with 5 degrees of freedom at a 95% confidence range, proving that the newly developed HPTLC and HPLC pharmacopoeial methods can be used interchangeably.The newly developed HPTLC method is easy, economical, specific, accurate, and roboust, thus it can be employed in a range of settings that require quality control and assurance activities of tetracycline hydrochloride (TC-HCl) in bulk and ointment dosage forms.