A Validated HPTLC Densitometric Method for The Quantitative Determination of Ubidecarenone in Bulk and in Capsule Formulation

A new, simple, precise, accurate and rapid high performance thin layer chromatographic method has been developed and validated for the estimation of ubidecarenone in bulk and in capsule formulation. The chromatographic separation was performed on aluminium TLC plates precoated with silica gel 60F254 as a stationary phase and methanol:water (7:3) as a mobile phase. Detection was performed densitometrically in the absorbance mode at 280nm for the evaluation of chromatograms. The system has given well sharp peak of ubidecarenone (Rf=0.51±0.02). The linearity of the method was established in the range of 1-6 ng/µL with correlation coefficient (r2) of 0.9995. The method was validated for precision, accuracy, robustness, ruggedness, LOD, and LOQ as per ICH guidelines. The limit of detection was found to be 0.0392 ng/µL, whereas the limit of quantitation was found to be 0.1189 ng/µL. The percentage label claim for ubidecarenone in the capsule formulation was found to be 99.96±0.4703. The accuracy of the method was confirmed by recovery studies. The percentage recovery was found to be in the range of 100.10-101.45% for ubidecarenone. The % RSD value was found to be less than 2. The low %RSD value indicates that there is no interference due to excipients used in the formulation. Hence, the developed method was found to be simple, precise, accurate, and rapid for the analysis of ubidecarenone in bulk and pharmaceutical formulation and it can be effectively applied for the quality control analysis of ubidecarenone in bulk and pharmaceutical formulation.

Knowledge and Attitude towards Label Claim and Health Benefits of Dark Chocolates among Customers of Oman—Cross-Sectional Survey

Dark chocolate is one of the most studied foods in the recent period due to its potential effects and health benefits. Admittedly, people's attitudes and acceptance of dark chocolate are still unknown. The cross-sectional study was aimed to determine the usage and effect of dark chocolate on health. It also aimed to study the attitude of young adults in Oman towards the consumption of dark chocolate and to discover the most preferred brands of DC in the Omani market. The study was conducted from spring 2020 to Fall 2021 in Oman. Two types of surveys were conducted. Firstly, a product survey was done to compare some brands according to the price, ingredient, expiry date, and country of origin. Secondly, across sectional-based survey was done focusing on the health benefits of consuming dark chocolate. Three hundred and forty-five (345) respondents participated in completing this survey. The results proved that many people are now aware of the health benefits of dark chocolate. The majority of the participants expressed their knowledge of the health aspect of dark chocolate and their interest in choosing the best product by examining the ingredients - especially the cocoa percentage- of the product before purchasing.

IN VITRO ASSESSMENT OF PHYSICOCHEMICAL PARAMETERS OF FIVE GENERICS AMLODIPINE BESYLATE TABLETS MARKETED IN YEMEN

Objective: The present paper aims to evaluate the quality of five different brands (local and imported) of oral film-coated tablets of generic Amlodipine besylate 5 mg marketed in Sana`a-Yemen, through physiochemical parameters. Methods: Different physicochemical parameters, including the uniformity of tablet weight, hardness, thickness, disintegration time, and an assay of active ingredients, were conducted to validate the quality of generics Amlodipine Besylate 5 mg according to USP specification. Results: From the obtained results, it was observed that all the brands of Amlodipine Besylate 5 mg have passed the tests and met the specifications of USP. Results of weight variation, hardness, thickness, and disintegration time were ranged from-3.8 % to+5.13 % to-1.25 % to+3.25 %, 5.06±0.31 to 13.21±1.5, 2.682±0.04 to 3.676±0.01 and 25 s to 2 min: 30 s, respectively. The dissolution test and the assay results of all the brands are also ranged within the acceptable label claim 93.7±2.24 to 98.4±0.85 and 93.22±0.38 to 100.15±0.33, respectively. However, there is no relation was found between the disintegration time and the dissolution test. Conclusion: According to the finding, all the selected Amlodipine Besylate 5 mg brands are met pharmacopeia standards and USP specifications. Therefore, the local and imported Amlodipine Besylate 5 mg can be used safely to get the desired therapeutic efficiency.

To Estimate the Label claim of tablet in their combination by simultaneous estimation using UV-Visible Spectrophotometric method

Objective: The main objective of the work was to check the label claim of tablet in combination by Simultaneous estimation by UV method. Method: Spectrophotometric method development and validation are plays important role in the development and manufacture of pharmaceuticals. This Spectrophotometric method was a simple and reproducible for the quantitative determination of Paracetamol and Caffeine in tablet formulation was developed and validated in the present work. The various parameters like specificity, linearity, precision, accuracy, robustness and ruggedness were studied according to ICH guidelines. The wavelength 273nm was selected for the estimation of Caffeine using distilled water as a solvent and the wavelength 243nm selected for the estimation of Paracetamol using distilled water as solvent the drug obeyed Beer’s-Lambert’s law over the concentration range 20-120µg/ml. Recovery study was performed to confirm the accuracy of the method. The method was successfully applied for routine analysis of this drug in formulation the method were validated as pr ICH guidelines. Conclusion: A simple UV spectrophotometric method was developed for the Simultaneous determination of Paracetamol and Caffeine in tablet formulation without any interference from the excipients. The present method succeeded in adopting a simple sample preparation that achieve satisfactory extraction recovery and facilitated its application in co formulated formulation.

Development and validation of pimavanserin tartrate by normal phase- HPTLC method

For the determination of pimvanserin tartrate in bulk and formulation, a rapid and simple High Performance Thin Layer Chromatography at 226 nm was developed and validated. The determination was carried out on thin coated aluminum backing plates covered with 200 mm layer of silica gel G 60 F254 (10×10 cm) plate as stationary phase and using a mobile phase of methanol: chloroform: trimethylamine (4:6:0.1 v/v/v) respectively. With a correlation coefficient (r) of 0.998, the development of pimvanserin tartrate was linear in the range of 0.7 to 4.2 µg/ml. The limit of detection (LOD) was found to be 7.68 ng/spot while the limit of quantification was found to be 23.28 ng/spot. The percentage label claim of pimvanserin tartrate in bulk and formulation was found to be 99 – 101 %. The percentage found in the formulation shows that no effect of excipient on drug. The conducted procedure has the benefit of being simple and quick. As a result, it can be used to examine pimvanserin tartrate in pharmaceutical formulations.

Quality Control of Vitamins A and E and Coenzyme Q10 in Commercial Anti-Ageing Cosmetic Products

Vitamins A and E and coenzyme Q10 are common ingredients in anti-ageing cosmetic products. Within this study, we evaluated the quality of commercial cosmetics with vitamin A (35 products), vitamin E (49 products), and coenzyme Q10 (27 products) by using validated HPLC–UV methods. Vitamin A was determined as retinol, retinyl palmitate, retinyl propionate, β carotene, and hydroxypinacolone retinoate in concentrations ranging from 950 ng/g to 19 mg/g. Total vitamin A contents, expressed with retinol equivalents, ranged from 160 ng/g to 19 mg/g, and were above the maximum concentration recommended by the SCCS in six of the 35 tested cosmetics. The content-related quality control of 10 cosmetics with specified vitamin A content revealed significant deviations (between 0% and 400%) of the label claim. Vitamin E was determined as both tocopherol and tocopheryl acetate in concentrations between 8.5 µg/g and 16 mg/g. Coenzyme Q10 was determined as ubiquinone in 24 tested cosmetics, which labelled it, in concentrations between 4.2 µg/g and 100 µg/g. Labelling irregularities were observed in all three active compound groups, resulting in a significant share (42%) of improperly labelled cosmetic products. The results of this study reveal the need for stricter cosmetics regulation and highlight the importance of their quality control, especially by evaluating the contents of the active compounds, in their efficacy and safety assurance.

Quantitative Spectrophotometric Estimation of Prednisolone in Tablet Dosage Form Using Eco-friendly Green Solvent and by applying Beer-Lambert’s Law Mathematical Equation Method

Prednisolone is a widely used synthetic glucocorticoid drug used in the treatment of allergies, inflammatory conditions, auto-immune disorders, acute and chronic obstructive pulmonary disease, rheumatoid arthritis, systemic lupus erythematosus, dermatitis, eye inflammation, asthma and multiple sclerosis. A simple and economical method was developed using eco-friendly green solvent. In this developed method the eco-friendly green solvent used was ethanol which is available easily. The method was projected to quantitative estimation and assay of Prednisolone in Prednisolone dispersible tablet dosage form. The amount and percent label claim of Prednisolone in tablet dosage form was estimated using Beer-Lambert’s law. Specific absorbance (A1%1cm) of Prednisolone is 415 at lambda max of 243 nm. The method developed was validated as per ICH guidelines. The proposed method was found to be simple, accurate, sensitive, precise, linear and rugged. The method obeys Beer-Lambert’s Law in the concentration range of 2.5-20μg/mL, as the r2 value was found to be 1.000. The mean percent recovery was found to be within acceptable range as per ICH guidelines. Hence the developed method can be used in regular quantitative analysis. The developed method acquires only one green solvent, low cost analytical equipment and the percent label claim can be calculated in the assay of Prednisolone tablets without using any standards solution or standard graph by just employing specific absorbance value in Beer-Lambert’s law, thereby concentration of drug can be calculated. As this method is simple, economical and eco-friendly it can be used elegantly and routinely in analytical laboratories and industries for estimation of Prednisolone in tablet formulation.

Multivariate optimization and evaluation of quaternary mixture in bulk and co-formulated dosage forms by central composite design

Background The current study describes the use of central composite design for multivariate optimization of resolution and retention time, taking into account different critical method parameters like organic phase, pH, flow rate, and wavelength for risk assessment. The chromatographic method for the assay of the most effective anti-viral regimen (EPCLUSA, DARVONI, and HARVONI) was developed. An experimental design was presented by sequential investigation of four independent parameters. The method was developed using XTERRA C18 (250 mm × 4.6 mm, 5 μm particle size) column in isocratic mode using potassium dihydrogen phosphate buffer (pH adjusted to 5) and acetonitrile (50:50 % v/v) as mobile phase at a flow rate of 1.0 ml/min and UV detection wavelength of 260 nm. Results The separation of four drugs with fine resolution and preferable retention times was achieved. Retention times of four drugs were found to be 2.96, 3.91, 7.15, and 11.94 min for daclatasvir, sofosbuvir, velpatasvir, and ledipasvir, respectively. The percentage accuracy of labelled claim was in the range of 99–102%, and the pooled %RSD for repeatability, precision, and accuracy was less than 2%. Conclusion The suggested method was applied for quantification and identification of studied drugs in tablets; the results agreed with the label claim and were validated according to the ICH guidelines. The optimized method can be used for pharmacokinetic and quality control studies.

CosG: A Graph-Based Contrastive Learning Method for Fact Verification

Fact verification aims to verify the authenticity of a given claim based on the retrieved evidence from Wikipedia articles. Existing works mainly focus on enhancing the semantic representation of evidence, e.g., introducing the graph structure to model the evidence relation. However, previous methods can’t well distinguish semantic-similar claims and evidences with distinct authenticity labels. In addition, the performances of graph-based models are limited by the over-smoothing problem of graph neural networks. To this end, we propose a graph-based contrastive learning method for fact verification abbreviated as CosG, which introduces a contrastive label-supervised task to help the encoder learn the discriminative representations for different-label claim-evidence pairs, as well as an unsupervised graph-contrast task, to alleviate the unique node features loss in the graph propagation. We conduct experiments on FEVER, a large benchmark dataset for fact verification. Experimental results show the superiority of our proposal against comparable baselines, especially for the claims that need multiple-evidences to verify. In addition, CosG presents better model robustness on the low-resource scenario.

Environment safe Method development and Validation of Dolutegravir in Bulk and Tablet dosage form by UV-Visible spectroscopy

To develop an environment-safe aqueous solubility enhancement method of poorly water-soluble drugs is the need of the pharmaceutical field. Because when organic solvents were used for solubility enhancement, there are many disadvantages like carcinogenicity, environment pollutant, flammable, toxicity, and cost. The hydrotropic method has been used to enhance the aqueous solubility of poorly water-soluble drugs. Dolutegravir is slightly soluble in water. To enhance aqueous solubility various hydrotropes were used and optimized the concentration of each hydrotrope. From these hydrotropes, a mixture of 10% sodium tricitrate and 10% sodium benzoate was selected because Dolutegravir was completely soluble in a mixed hydrotropic solution. Method development and analytical validation were performed. The maximum wavelength of Dolutegravir in the hydrotropic mixture was found a 268nm, and the linearity curve in the range of 5-25µg/ml. A regression coefficient was found to be 0.999. Percent label claim, accuracy (% RSD) were found 99.58%, 0.13(80%), 0.11(100%), 0.13(120%), respectively. The LOD for Dolutegravir was determined to be 0.037μg/ mL, and LOQ was found to be 0.11μg/mL.