Analytical Method Development and Validation for Related Substance in Iguratimod by HPLC (original) (raw)
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International Journal of Pharmacy and Pharmaceutical Sciences
Objective: The objective of the work was to develop and validate stability indicating HPTLC method for the estimation of Iguratimod. Methods: The method employed HPTLC aluminium pre-covered silica gel 60 GF254 plates (10 cm × 10 cm with 250 μm layer thickness) as stationary phase while the solvent system was n-Hexane: Ethyl Acetate (5:5 v/v) with densitometric scanning at 256 nm. Sample was applied as a band of 8 mm width using Camag 100 μl sample syringe (Hamilton, Switzerland) using a linomat 5 applicator (Camag, Switzerland). Migration distance was 80 mm. Further the sample was subjected for stress conditions under acid and base hydrolysis, oxidation, thermal, neutral and photolytic conditions. Method validation done according to ICH Q2 (R1) guidelines. Results: Retention factor (Rf) of the drug was 0.41±0.02. The linearity of the method was found to be within the concentration range of 200-1200 ng/band with R2= 0.983. Limit of detection and limit of quantification were found to ...
Journal of emerging technologies and innovative research, 2018
A simple reverse-phase HPLC method for the estimation of Azelastine hydrochloride in nasal spray formulations has been developed. The method is simple, accurate, precise, specific and linear over the analysis range. This developed method has been validated according to International Conference on Harmonization (ICH) guideline with respect to system suitability, specificity, precision, linearity, accuracy, and robustness. An isocratic condition of mobile phase comprising Phosphate buffer (pH 3.1): Acetonitrile in a ratio of 60:40, v/v at a flow rate of 1.0 mL/minute over RP C18 (octadecylsilane (ODS), 250 × 4.6 mm, 5 µm, CHROMOSIL) column at ambient temperature was maintained. Besides, the chromatographic peak was observed sharp & symmetric. The proposed method was successfully applied for the estimation of the Azelastine hydrochloride in nasal spray formulation.
International Journal of Pharmacy and Pharmaceutical Sciences, 2022
Objective: The objective of the work was to develop and validate stability indicating HPTLC method for the estimation of Iguratimod. Methods: The method employed HPTLC aluminium pre-covered silica gel 60 GF254 plates (10 cm × 10 cm with 250 μm layer thickness) as stationary phase while the solvent system was n-Hexane: Ethyl Acetate (5:5 v/v) with densitometric scanning at 256 nm. Sample was applied as a band of 8 mm width using Camag 100 μl sample syringe (Hamilton, Switzerland) using a linomat 5 applicator (Camag, Switzerland). Migration distance was 80 mm. Further the sample was subjected for stress conditions under acid and base hydrolysis, oxidation, thermal, neutral and photolytic conditions. Method validation done according to ICH Q2 (R1) guidelines. Results: Retention factor (Rf) of the drug was 0.41±0.02. The linearity of the method was found to be within the concentration range of 200-1200 ng/band with R 2 = 0.983. Limit of detection and limit of quantification were found to be 34.69 and 105.12 ng/band respectively. The % mean recovery was found to be 100.38±0.83. Stress results showed that there is degradation in acid and base conditions but two degradant peaks were observed only under alkaline stress condition Conclusion: The developed method found to be accurate, simple and precise. Method is successfully employed for quantification of the drug under various stress conditions.
New stability indicating reverse phase high performance liquid chromatography (HPLC) method is developed for the determination of Imiquimod and its impurities. Separation is achieved on a C18 column (Inertsil-ODS3 4.6 × 250 mm, 5 µm) using gradient elution mode with mobile phase-A having disodium hydrogen phosphate buffer (10 mM) with 0.1% v/v triethyl amine and pH adjusted to 6.0 with ortho-phosphoric acid while mobile phase-B consist of an equal mixture of methanol and acetonitrile. The flow rate was optimized to 1.2 mL/min and column oven temperature 30°C. Detection was carried out at wavelength 226 nm. This developed method is then validated as per International Council for Harmonisation (ICH) guideline and found out to be linear, accurate, specific, selective, precise, and robust. The drug is also subjected to forced degradation using Original Research Article
IJARW, 2020
Indapamide is a Thiazide like diuretic drug which is used in treatment of Hypertension, as well as in edema, Heart attack, stroke and heart failure in persons with high blood pressure. It is available as single component and multicomponent in marketed formulations. This article aims to study comprehensively about the previously reported various analytical methods used in determination of Indapamide.The various analytical method including in the analysis of indapamide are chromatographic method, LC-MS (Liquid Chromatography-mass spectroscopy), GC-MS (Gas chromatography-mass spectroscopy),spectrofluorometric and UV Visible spectrophotometry techniques for estimation of Indapamide in biological samples, bulk and pharmaceutical formulation.
2010
Itopride hydrochloride is a benzamide derivative in the class of prokinetic drugs. it has been approved for the symptomatic treatment of disorders like non-ulcer dyspepsia. chronic gastritis , diadetic gastro paresis or functional dyspepsia. the present study was designed to study the method of development in pharmaceutical dosage forms by reversed hplc. through developed validation method we can analyse the drug in reversed phase pharmaceutical dosage form by hplc. validation is a constant evolving process that starts before an instrument is placed on line and continuous long after method development and transferred. here a new hplc method for itopride hydrochloride and rabeprazole sodium was developed and validated the same. the best chromatographic seperation was performed on phenomenex c 18 column and the uv detection wave length was set at 268nm. the mobile phase used was methanol : water : acetonitrile (50:40:10). the retention time of itopride hydrochloride and rabeprazole so...
A series which presents the current state of the art of chosen sectors of analytical chemistry. Written at professional and reference level, it is directed at analytical chemists, environmental scientists, food scientists, pharmaceutical scientists, earth scientists, petrochemists and polymer chemists. Each volume in the series provides an accessible source of information on the essential principles, instrumentation, methodology and applications of a particular analytical technique.
2016
The aim of the present study was to develop a sensitive chromatographic method by using HPLC with UV detector for quantitative determination of imidacloprid (insecticide) in multiple modes of products available in market. For the separation of analyte, C-18 beckman column (5μm x 0.46cm x 15cm) was used as stationary phase, whereas acetonitrile and water (70:30 v/v) was suitably used as mobile phase. For the optimization of method, different associated parameters were also investigated those may influence the efficiency of separation. Pump was adjusted to flow at 1mL/min. throughout the analysis was performed at ambient temperature and 270nm wavelength. Linearity of the chromatographic results was checked between the range of 0.5 to 300μg/mL and R was found to be 0.999. LoD and LoQ of the method were found to be 4 and 2 12μg/mL respectively and the reliability of the method was found to be good; up to the concentration level of 300μg/mL. Method validation tests ensured the proposed m...
2013
A simple isocratic RP-HPLC stability indicating method has been developed and subsequently validated for the determination of Irinotecan HCl and its related substance (SN-38) in pharmaceutical dosage forms as per ICH guidelines. The separation achieved on a reversed phase Phenomenex Luna C 18 Column (5µ, 250 × 4.60 mm) as a stationary phase and 0.5% trichloro acetic acid: Acetonitrile: Methanol (60: 20: 20 v/v/v) as mobile phase at a flow rate of 1.0 ml/min. The UV detection was performed at 372 nm. The retention time for Irinotecan HCl and SN-38 was found to be 8.65 and 7.30 min respectively. The detector response was linear in the concentration range of 30-150 µg/ml. The respective linear regression equation being Y= 5233.x + 13299 with R 2 = 0.999. The percentage of Irinotecan HCl in pharmaceutical dosage form was found to be 100.5% and the percentage of related substance (SN-38) in formulation was found to be 0.19%. The limit of detection and the limit of quantification were found to be 0.014 µg/ml and 0.045 µg/ml respectively. The results of the study showed that, the proposed RP-HPLC method was simple, rapid, precise, accurate and stability indicating, which can be used for the routine determination of Irinotecan HCl and its related substance (SN-38) in pharmaceutical dosage form.