scholarly journals DEVELOPMENT AND VALIDATION OF STABILITY INDICATING METHOD RP-HPLC METHOD OF ACOTIAMIDE

2018 ◽  
Vol 10 (9) ◽  
pp. 1 ◽  
Author(s):  
Charu P. Pandya ◽  
Sadhana J. Rajput
Keyword(s):  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Rp Hplc ◽  
Acid And Base ◽  
Stress Degradation ◽  
Development And Validation ◽  
Tablet Dosage

Objective: The objective of present work was to develop and validate simple, precise, accurate and specific stability indicating method for determination of acotiamide in presence of its degradation products.Methods: An isocratic RP-HPLC method has been developed using C-8 Thermo Hypersil BDS Column (250 x 4.6 mm i.d., 5µparticle size) with the mobile phase composition of acetonitrile: 0.1 % triethylamine in 0.2% formic acid (30: 70) at column oven temperature of 40 °C. The flow rate was 1.0 ml min-1 and effluent was detected at 282 nm. The method was validated in terms of linearity, accuracy, precision, LOD (Limit of Detection), LOQ (Limit of Quantification) and robustness as per ICH guidelines.Results: The method was found to be linear in the range of 10-60µg/ml. Limit of detection and limit of quantification was found to 0.36µg/ml and 1.10 µg/ml.% Recovery was found to be in the range of 99.45%-99.75%and precision less than 2%. The developed method was successfully applied for estimation of Acotiamide in marketed tablet formulation and percentage assay was found to be 100.45%. Acotiamide was subjected to stress degradation under acid, base, neutral hydrolysis, oxidation, dry heat, photolysis conditions. Significant degradation was observed in acid and base degradation.Conclusion: The developed RP-HPLC method was simple, rapid, accurate, precise and stability indicating for the estimation of Acotiamide in bulk and tablet dosage form.

NEW STABILITY INDICATING METHOD FOR ESTIMATION OF PURITY OF FLIBANSERIN ACTIVE PHARMACEUTICAL INGREDIENT

INDIAN DRUGS ◽  
2020 ◽  
Vol 57 (04) ◽  
pp. 40-44
Author(s):  
Yik-Ling Chew ◽  
◽  
Hon-Kent Lee ◽  
Subrahmanya Lokesh Bontha Venkata
Keyword(s):  
Ammonium Acetate ◽  
Limit Of Detection ◽  
Sexual Interest ◽  
Active Pharmaceutical Ingredient ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Rp Hplc ◽  
Ich Guidelines

Flibanserin has been recently approved by the USFDA for treating female sexual interest disorder. It is currently not included in any of the Pharmacopoeias. No stability indicating method information about flibanserin has been reported in the literature. Flibanserin stock solution (1 mg/mL) was prepared and serially diluted (concentration ranged 1-20 μg/mL). Flibanserin solutions (1-20 μg/mL) were analysed using RP-HPLC under isocratic elution of mobile phase acetonitrile and ammonium acetate (60:40; V/V) at 1 mL/minute. This HPLC method was validated for linearity, accuracy, precision, robustness, limit of detection (LOD) and limit of quantification (LOQ), according to ICH guidelines. Results showed that the method developed has promising linearity (r2= 0.9993), accuracy, precision (0.92-1.61%), robustness, LOD and LOQ. The developed HPLC method for evaluation of flibanserin was found reliable, precise, sensitive, accurate and repeatable for routine analysis and quality control of flibanserin. It is suitable to be used as stability indicating method in pharmaceutical analysis.

Development and validation of a stability-indicating RP-HPLC method for simultaneous determination of dapagliflozin and saxagliptin in fixed-dose combination

2018 ◽  
Vol 42 (4) ◽  
pp. 2459-2466 ◽  
Author(s):  
N. Singh ◽  
P. Bansal ◽  
M. Maithani ◽  
Y. Chauhan
Keyword(s):  
Hplc Method ◽  
Fixed Dose ◽  
Simultaneous Estimation ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Rp Hplc ◽  
Dose Combination ◽  
Development And Validation ◽  
Tablet Dosage

A simple and precise stability indicating method for the simultaneous estimation of dapagliflozin and saxagliptin in combined tablet dosage form was developed and validated using RP-HPLC.

scholarly journals Development and validation of Stability Indicating HPLC method for estimation of Embelin in Embelia tsjeriam cottam(Vidanga)

2015 ◽  
Vol 6 (3) ◽  
Author(s):  
Sweta V Kulkarni ◽  
Mrinalini C Damle
Keyword(s):  
Mobile Phase ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Good Recovery ◽  
Uv Detector ◽  
Limit Of Quantification ◽  
Stability Indicating ◽  
Stress Degradation ◽  
Development And Validation ◽  
Insight Into

           Embelin, is an active phytoconstituent obtained from fruits of Embelia tsjeriam cottam, commonly known as Vidanga. A simple stability indicating HPLC method for the estimation of Embelin has been developed and validated as per ICH Q2A(R1). Sample was eluted using HiQsil C8 (4.6mm×250mm) column. The mobile phase consisted of Methanol: Acetonitrile: 1% O-phospheric acid in water in the ratio of 70:15:15 v/v/v which was sonicated to degas and delivered at a flow rate of 1ml/min at ambient temperature. The retention time of Embelin was 6.05 ± 0.2 minutes. Studies were performed using an HPLC system equipped with a UV detector; the response was monitored at 291 nm. A good linear relationship over the range of 2–10 µg/ml concentrations with correlation coefficient value of 0.999 was obtained. The accuracy of the method is indicated by good recovery in the range of 98.9-101.2 % and precision less than 2% RSD. The limit of detection and limit of quantification were found to be 0.47 and 1.44µg/ml respectively. Embelin was subjected to stress conditions as per ICH Q2A(R2) and a significant degradation was found to occur by acid hydrolysis, oxidation and thermal stress. Stress degradation studies on embelin provide an insight into its stability. 

scholarly journals Development and Validation of a Rapid RP-HPLC Method for the Estimation of Esmolol Hydrochloride in Bulk and Pharmaceutical Dosage Forms

2010 ◽  
Vol 7 (3) ◽  
pp. 807-812 ◽  
Author(s):  
Vanita Somasekhar ◽  
D. Gowri Sankar
Keyword(s):  
Limit Of Detection ◽  
Hplc Method ◽  
Detector Response ◽  
Reverse Phase Hplc ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Accuracy And Precision ◽  
Development And Validation

A reverse phase HPLC method is described for the determination of esmolol hydrochloride in bulk and injections. Chromatography was carried on a C18column using a mixture of acetonitrile, 0.05 M sodium acetate buffer and glacial acetic acid (35:65:3 v/v/v) as the mobile phase at a flow rate of 1 mL/min with detection at 275 nm. The retention time of the drug was 4.76 min. The detector response was linear in the concentration of 1-50 μg/mL. The limit of detection and limit of quantification was 0.614 and 1.86 μg/mL respectively. The method was validated by determining its sensitivity, linearity, accuracy and precision. The proposed method is simple, economical, fast, accurate and precise and hence can be applied for routine quality control of esmolol hydrochloride in bulk and injections.

scholarly journals LC-MS characterization of acid degradation products of metoclopramide: Development and validation of a stability-indicating RP-HPLC method

2020 ◽  
Vol 11 (1) ◽  
pp. 781-789
Author(s):  
Sriram Valavala ◽  
Nareshvarma Seelam ◽  
Subbaiah Tondepu ◽  
Suresh Kandagatla
Keyword(s):  
Liquid Chromatography ◽  
Mobile Phase ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Hplc Technique

The present study aims to develop a simple, accurate and specific stability-indicating RP-HPLC technique for the analysis of metoclopramide in the presence of its stress degradation products and characterization of degradation compounds by LC-MS/MS analysis. As per ICH Q1A-R2 guidelines, the drug was exposed to acid hydrolytic stress condition. Three degradation products were formed for MCP in acid hydrolysis. The liquid chromatography was processed on a Luna C18-(2) 100A,250×4.6mm 5micron column using an isocratic mobile phase consisting of 0.1% formic acid in water-acetonitrile (20:80, v/v) by adjusting the mobile phase at 1 ml/min flow rate with wavelength detection at 273 nm. The developed procedure was applied to LC-MS/MS (liquid chromatography-tandem mass spectrometry) for the characterization of all the degradant components. Total new three degradation compounds were recognized and identified by LC-MS/MS. The developed RP-HPLC technique was validated as per the ICH Q2-R1 guidelines. Limit of detection and limit of quantification values of MCP were evaluated from the linearity graph and were found to be 5.23 µg/ml and 17.44 µg/ml. Accuracy study was established at 80.0, 100.0 and 120.0 µg/ml concentration levels and the findings were found in the range of 98.4% - 101.8%. The linearity of the technique was assessed over the drug concentration range of 50.0 µg/ml to 250.0 µg/ml and the regression equation, slope and correlation coefficient values were found to be y = 10618x + 1623.2, 10618 and 0.9996 respectively. The developed technique was uninterruptedly applied for the quantification of metoclopramide inactive pharmaceuticals.

scholarly journals Development and Validation of Stability Indicating RP-HPLC Method for the Estimation of Cinacalcet Hydrochloride in Bulk and Their Formulations

2020 ◽  
Vol 10 (6) ◽  
pp. 6610-6618
Keyword(s):  
Dosage Forms ◽  
Hplc Method ◽  
Forced Degradation ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Cinacalcet Hydrochloride ◽  
Development And Validation ◽  
Tablet Dosage

A Simple, selective, accurate, precise, linear, and stability-indicating RP-HPLC method was developed and validated for the estimation of Cinacalcet hydrochloride in bulk and tablet dosage forms. Chromatographic separation was achieved on X-Terra Symmetry C18 (4.6 x 150mm; 5 m) with mobile phase containing Phosphate buffer: Acetonitrile (40:60 v/v) pH adjusted to 3.0 ±0.05 with diluted ortho-phosphoric acid. The flow rate was maintained at 0.9 mL/min. The eluent was monitored at 282 nm. Moreover, the retention time of Cinacalcet was 2.8 minutes. The method was validated for linearity, accuracy, precision, and robustness as per ICH guidelines. The developed method was found linear between 25-150 μg/ml, and the linear regression coefficient was 0.999. The % RSD values are less than 2 % indicating the accuracy and precision of the method. The percentage of recovery was obtained from 98-102%. The system suitability parameters were found to be within the limit. Forced degradation studies were conducted under various conditions. The proposed method is simple, rapid, precise, and accurate. It can be used for the quantitation of Cinacalcet hydrochloride in bulk and commercial pharmaceutical dosage forms.

scholarly journals RP-HPLC Method Development and Validation for the Estimation of Mirabegron in Bulk and Dosage Form

2020 ◽  
Vol 10 (1) ◽  
pp. 31-38
Author(s):  
Rahul Suryawanshi ◽  
Siddiqua Shaikh ◽  
Snehal Patil
Keyword(s):  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Limit Of Quantification ◽  
Rp Hplc ◽  
Hplc Method Development ◽  
Tablet Dosage

A new, simple, precise, accurate and reproducible Reverse Phase High Performance Liquid Chromatography (RP-HPLC) method for Simultaneous estimation of bulk and pharmaceutical formulations. Separation of Mirabegron was successfully achieve , C18, 250X4.6mm, 5µm or equivalent in an isocratic mode utilizing methanol water (70:30) at pH 5.0 Adjusted to OPA at a flow rate of 1.0ml/min and eluate was monitored at 243nm, with a retention time of 2.584 minutes for Mirabegron. The method was validated and the response was found to be linear in the drug concentration range of 50µg/ml to150 µg/ml for Mirabegron. The values of the correlation coefficient were found to 0.999for Mirabegron. The Limit of Detection(LOD) and Limit of Quantification (LOQ) for Mirabegron were found to be 0.149 and 0.498 respectively. This method was found to be good percentage recovery were found to be 99 indicates that the proposed method is highly accurate. The specificity of the method shows good correlation between retention times of standard with the sample so, the method specifically determines the analyte in the sample without interference from excipients of tablet dosage forms. The method was extensively validated according to International Council for Harmonisation(ICH) guidelines for Linearity, Accuracy, Precision, Specificity and

Stability Indicating Method for known and unknown impurities profiling for Vildagliptin in Vildagliptin Tablet

2020 ◽  
Vol 17 ◽  
Author(s):  
Nitin Mahajan ◽  
Mazhar Farooqui ◽  
Suparna Deshmukh
Keyword(s):  
Degradation Products ◽  
Hplc Method ◽  
Alkaline Stress ◽  
Limit Of Quantification ◽  
Stability Indicating ◽  
Oral Antihyperglycemic Agents ◽  
Stability Indicating Method ◽  
Rp Hplc ◽  
Triethyl Amine

Background: Vildagliptin is a drug for the treatment of diabetes. DPP-IV inhibitor represents a new class of oral antihyperglycemic agents to treat patients with type 2 diabetes. Several RP-HPLC method reported for determination of Vildagliptin alone. However, it was noticed that no stability indicating method is available in any Pharmacopeia (USP/BP/EP/JP) or in any literature for quantification of known and unknown impurities profiling for Vildagliptin in Vildagliptin tablets. Objective: The aim of this study to develop a simple, sensitive, rugged, robust and specific novel gradient stability indicating RP-HPLC method for quantitative determination of known, unknown impurities and degradants of Vildagliptin in Vildagliptin Tablets. Methods: Chromatographic separation has been achieved on Hypersil ODS column (250 x 4.6) mm, 5 μm with mobile phase consisting mixture of Perchloric acid Buffer, methanol, acetonitrile and Triethyl amine delivered at flow rate of 1.0 mL minute-1 and the detection wavelength 210 nm. The developed method was validated as per ICH guidelines. Results: Vildagliptin was found degraded significantly under oxidative and alkaline stress condition. The degradation products were well resolved from Vildagliptin and its impurities. Analytical Method found Linear, accurate and precise from LOQ (Limit of Quantification) level to 150 % of impurity specification limit (0.5 %). Conclusion: The method found sensitive, rapid and accurate quantification of known, unknown impurities and degradants. The peak purity results confirmed that the Vildagliptin peak was homogeneous and pure in all stress samples, thus proving the stability indicating nature of the method.

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