ICH guidelines

This research introduces a straightforward, rapid, sensitive, and selective analytical method for measuring daprodustat in both bulk powder and tablet forms. The techniques used include UV-Visible spectrophotometry and reversed-phase high-performance liquid chromatography (RP-HPLC). For the UV-Visible method, a Systonic AU-2702 double-beam spectrophotometer was used to measure Daprodustat 's absorbance at 265 nm. The RP-HPLC procedure employed a Shimadzu SPD-10A C18 column (250×4.6 mm, 5 µm). The mobile phase consisted of a mixture of acetonitrile and distilled water (70:30, v/v), with 0.1% formic acid added. Key operational parameters included a flow rate of 1.2 mL/min, an injection volume of 10 μL, and a column temperature of 30 °C. The method's linearity ranged from 10 to 100 μg/mL. The entire procedure was validated following ICH Q2 (R1) guidelines, confirming its specificity, linearity, sensitivity, precision, accuracy, robustness, and system suitability. The technique yields highly sensitive results, with Limits of Detection (LODs) and Limit of Quantification (LOQs) of 0.6174 μg/mL and 1.87μg/mL for daprodustat. Recovery rates ranged from 98% to 102%, and both intra-day and inter-day precision (measured by % RSD) were below 2%. The method demonstrated excellent specificity, avoiding interference from excipients or formulation matrices. Overall, this study provides a complete analytical framework applicable for routine pharmaceutical analysis, ensuring quality control, safety assessment, and regulatory compliance for daprodustat.   

This study reports the method development and validation for anti-diabetic drugs by UPLC.  A new, simple, rapid, selective, precise and accurate ultra performance liquid chromatography assay has been developed for simultaneous estimation of Remogliflozin, Vildagliptin and Metformin. The separation was achieved by using ODS 3V column with dimensions 5 µm, 4.6 mm x 250 mm. The pH of mobile phase was adjusted to 4.5 with acetonitrile. The flow rate was 0.4 mL/min, and the separated drugs were detected using UPLC detector at the wavelength of 260 nm. The method was validated as per ICH guidelines. The proposed method was found to be accurate, reproducible, and consistent. It was successfully applied for the analysis of these drugs in marketed formulations and could be effectively used for the routine analysis of formulations.

A muscle spasm, or muscle cramp, is an involuntary contraction of a muscle. Muscle spasms occur suddenly, usually resolve quickly, and are often painful. The use of NSAIDs has been routine in the management of muscle spasm. Although effective at reducing pain and inflammation. NSAIDs may not be appropriate to use frequently or longer time due to their known side effects. Natural agents like camphor and menthol are having analgesic activity as well as each active individual ingredient has its own medicinal value. For greater and effective results we are using combination of camphor and menthol. Hydrophilic and hydrophobic ointments were prepared by taking 25mg, 50mg and 100mg of each agent as combination of camphor-menthol. All the prepared formulations were evaluated for pH, spreadability and diffusion studies. The selected formulations were evaluated for In-vivo studies in comparison with marketed preparations. The finalized preparation was kept for stability studies according to ICH guidelines.

The present work deals with the development of reliable method for the estimation of pioglitazone hydrochloride by using UV spectroscopy. The pioglitazone hydrochloride showed absorption maxima at wavelength 268nm respectively. The linearity range for pioglitazone hydrochloride was in the range of 10-50μg/ml with correlation coefficient of 0.999. The precision was carried out for pioglitazone hydrochloride and value was found to be less than 2. The proposed method’s results were found satisfactory and are suitable for determination of pioglitazone hydrochloride for routine quality control of drug in bulk and formulation. This method is validated according to ICH guidelines Q2R1. Keywords: Pioglitazone hydrochloride, ICH guidelines, validation, method development.  

The objective of present work was to develop and validate a rapid reverse phase high-performance liquid chromatography (RP-HPLC) method for the quantitative analysis of lenvatinib in bulk and pharmaceutical dosage forms. Chromatographic analyses were performed on an ODC column of 250mm 4.6mm: i.d and 5µ particle size with a mobile phase comprising of 0.5M ammonium acetate and acetonitrile in the ratio 90:10 v/v. The   flow rate maintained at 1 ml/min, detected lenvatinib at RT 1.15 minutes. The lenvatinib was detected and quantitated using a photodiode array detector at a wavelength of 367 nm. The method was shown to be specific and linear in the range of 20-120?g/ml (r2= 0.999). The precision (intra- and inter-day) was demonstrated. The method is robust relative to changes in flow rate, column and temperature. The limits of detection and quantitation were 0.4 and 0.12µg/ml respectively. Validation parameters such as specificity, linearity, precision, accuracy, and robustness, limit of detection (LOD) and limit of quantitation (LOQ) were evaluated for the method according to the International Conference on Harmonization (ICH) Q2 R1 guidelines. The method fulfilled the requirements for reliability and feasibility for application to the quantitative analysis of lenvatinib in bulk and pharmaceutical dosage forms.

The objective of this work was to develop a simple, sensitive, accurate, precise and reproducible high performance liquid chromatography (HPLC) method for the determination of salicylic acid in pharmaceutical dosage forms. Shimadzo Prominance model L20 AD HPLC system equipped with SPD 20A UV-Vis detector was used for the analysis. The separation was done on RESTEX allure C18 column (3 μm, 15 cm × 4.6 mm), for an isocratic elution a mixture of water, methanol and glacial acetic acid (65:35:1, v/v) mobile phase at a wavelength of 254 nm. The flow rate was 1.0mL/min. The RP-HPLC method developed for analysis of salicylic acid was validated with respect to specificity, selectivity, linearity, accuracy, precision and robustness as per the ICH guidelines. The retention time of salicylic acid was 7.575 min. The linearity was established over the concentration ranges of 50-350 μg/mL with correlation coefficients ( r2) 0.999.  The percentage accuracy of salicylic acid ranged from 99.76 -101.66%. The relative standard deviation values for intra-day and inter-day precision was lower than 2.0% and the assay result was found to be in the range 99.57-101.32%. Salicylic acid was subjected to stress conditions such as neutral, acidic, alkaline, oxidation and photolysis degradations as per ICH guidelines. The degradation studies revealed that the drug was found to degrade maximum (1.67%) in alkaline degradation conditions and was highly resistant towards neutral, acidic, oxidative and photolytic degradation conditions.

The article aims at developing simple, fast and effective dissolution method for Dabigatran etexilate mesylate capsules by RP-HPLC and validate as per ICH guidelines. The optimized RP-HPLC method for dissolution studies uses a reverse phase column, Phenomenex Luna C18 (250 X 4.6 mm;5μ), a mobile phase of triethylammonium phosphate buffer (pH 3.0):acetonitrile in the proportion of 40:60 v/v, diluent as 0.01N HCl, flow rate of 1.0ml/min, injection volume as 20µl. and a detection wavelength of 341nm using a UV detector. The optimized dissolution conditions include, 0.01N HCl as dissolution media, apparatus as USP Type 1 Basket, rpm as 100, dissolution media temperature as 37±0.5ºC, dissolution volume as 500ml, dissolution time point as 30mts, working concentration of standard and sample as 5µg/ml and a detection wavelength of 341 nm. The developed method resulted in Dabigatran etexilate exhibiting linearity in the range 1.25-10μg/ml. System precision and intra-day precision is exemplified by relative standard deviation of 1.59% and 2.21% respectively. Method was found to be rugged/inter day precise as %RSD was found to be 3.25. Percentage Mean recovery was found to be greater than 80% at all the three levels by absolute method during accuracy studies. LOD and LOQ for Dabigatran etexilate were found to be 0.05ng/ml and 5ng/ml respectively. Hence it can be concluded that effective dissolution method by RP-HPLC is developed and validated as per ICH guidelines which can be applicable in various pharmaceutical industries.

A specific and accurate HPLC method is developed for the determination of etoposidein bulk drugs and in solid capsule dosage form. Best symmetric peak shape obtained with Inertsil ODS C-18 column (250 X 4.6 mm, 5μ) column in an isocratic mode, with retention time 5 min.The mobile phase used was Water : Acetonitrile  60:40(v/v)with flow rate 1.0 ml/min and effluent was monitored at 263 nm. As per ICH guidelines method has validated. Method has found linear in the range of 5-45 µg/ml. The LOD and LOQ were found to be 0.02 and 0.06 µg/ml respectively. Method was found specific with respective of diluents, excipients and degradants.

A simple, rapid, precise, and economical spectrophotometric method has been developed for quantitative analysis of Rilpivirine hydrochloride (RILH) in manufactured tablet formulations. The initial stock solution of RILH was prepared in dimethyl formamide: acetonitrile solvent and subsequent dilution were done in acetonitrile. The standard solution of RILH in acetonitrile showed absorption maxima at 281.6 nm. The drug obeyed Beer–Lambert’s law in the concentration range of 1–16 μg/mL with coefficient of correlation (R2) was 0.9999. It showed coefficient of variation below 2 % in intra-run and inter-run precision.  The results of analysis have been validated as per ICH guidelines. The method can be adopted in routine analysis of RILH in bulk and tablet dosage form and it involves relatively low cost solvents and no complex extraction techniques.

To assure the quality of drugs, impurities must be monitored carefully. It is important to understand what constitutes an impurity and to identify potential sources of such impurities. Selective analytical methods need to be developed to monitor them. It is generally desirable to profile impurities to provide a yardstick for comparative purposes. New impurities may be observed as changes are made in the synthesis, formulation, or production procedures, albeit for improving them. At times it is necessary to isolate and characterize an impurity when hyphenated methods do not yield the structure or when confirmation is necessary with an authentic material. Availability of an authentic material can also allow toxicological studies and provide a standard for routine monitoring of the drug product.