Concurrent Determination of Daclatasvir and Sofosbuvir in Pure Binary Mixture and Their Combined Film Coated Tablets by a Simple Stability Indicating RP-HPLC Method

2021 ◽  
pp. 5913-5918
Author(s):  
Ramreddy Godela ◽  
Sowjanya G
Keyword(s):  
Degradation Products ◽  
Hplc Method ◽  
Forced Degradation ◽  
Good Resolution ◽  
Stability Indicating ◽  
Extreme Stress ◽  
Rp Hplc ◽  
Highly Sensitive ◽  
Validation Parameters ◽  
Acid And Base

A trouble-free, simple, specific and highly sensitive stability indicating phase HPLC method was developed for concurrent assessment of Daclatasvir and Sofosbuvir in pure and in their combined tablet formulation. An effectual separation was accomplished by using XDB Phenyl (250 x 4.6mm, 5µ,100 A0) column, mobile phase composition of Acetonitrile: buffer(0.1%v/v Trifluoroaceticacid in water) (50:50 v/v) and isocratic elution at a flow rate of 1ml/min and detection wavelength of 275nm. The extreme stress conditions like hydrolysis with acid and base, peroxide oxidation, thermal decomposition were used as per ICH specifications to assess the stability of the analytes in bulk and dosage forms. The retention times of Daclatasvir and Sofosbuvir were found at 2.8 and 3.7min respectively. The proposed method has linear response in the concentration ranges from 12 to 36µg/ml and 80 to 240 µg/ml for Daclatasvir and Sofosbuvir respectively. The detection and quantification limits calculated as 2.5μg/ml and 7.8μg/ml for DCL, 5.2μg/ml and 15.8μg/ml SOF respectively. All the method validation parameters were met the acceptance limits of Q2 specifications of ICH procedures. The degradation products produced by forced degradation studies were have good resolution from Daclatasir and Sofosbuvir peaks, which represents the methods stability. The proposed RP-HPLC method was highly sensitive, precise, stability indicating and economical. That’s why the method has the capacity to employ in the pharmaceutical manufacturing of Daclatasvir and Sofosbuvir and routine analysis in quality control department.

scholarly journals Validated Stability Indicating RP-HPLC Method for Simultaneous Estimation of Codeine Phosphate and Chlorpheniramine Maleate from Their Combined Liquid Dosage Form

2013 ◽  
Vol 2013 ◽  
pp. 1-7 ◽  
Author(s):  
Ramakrishna Kommana ◽  
Praveen Basappa
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Codeine Phosphate ◽  
Chlorpheniramine Maleate ◽  
Combination Drug ◽  
Stability Indicating ◽  
Rp Hplc

The present paper describes the development of quick stability indicating RP-HPLC method for the simultaneous estimation of codeine phosphate and chlorpheniramine maleate in the presence of its degradation products, generated from forced degradation studies. The developed method separates codeine phosphate and chlorpheniramine maleate in impurities/degradation products. Codeine phosphate and chlorpheniramine maleate and their combination drug product were exposed to acid, base, oxidation, dry heat, and photolytic stress conditions, and the stressed samples were analysed by proposed method. The proposed HPLC method utilizes the Shimadzu HPLC system on a Phenomenex C18 column (, 5 μ) using a mixture of 1% o-phosphoric acid in water : acetonitrile : methanol (78 : 10 : 12) mobile phase with pH adjusted to 3.0 in an isocratic elution mode at a flow rate of 1 mL/min, at 23°C with a load of 20 μL. The detection was carried out at 254 nm. The retention time of codeine phosphate and chlorpheniramine maleate was found to be around 3.47 min and 9.45 min, respectively. The method has been validated with respect to linearity, robustness, precision, accuracy, limit of detection (LOD), and limit of quantification (LOQ). The developed validated stability indicating HPLC method was found to be simple, accurate, and reproducible for the determination of instability of these drugs in bulk and commercial products.

scholarly journals DEVELOPMENT AND VALIDATION OF STABILITY INDICATING RP-HPLC METHOD FOR DETERMINATION OF β-ACETYLDIGOXIN

2016 ◽  
Vol 9 (1) ◽  
pp. 54
Author(s):  
Megha Sharma ◽  
Neeraj Mahindroo
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Hplc Method ◽  
Stability Study ◽  
Array Detector ◽  
Forced Degradation ◽  
Simple Method ◽  
Stability Indicating ◽  
Rp Hplc

Objective: The objective of the present study was to develop and validate a novel stability indicating reverse phase-high performance liquid chromatography (RP-HPLC) method for determination of β-acetyldigoxin, an active pharmaceutical ingredient (API).Methods: The chromatographic separation was carried out on Agilent Technologies 1200 series HPLC system equipped with photo diode array detector and C-18 (4.6x250 mm, 5 µ) column. The mobile phase consisted of water: acetonitrile (65:35 v/v), delivered at a flow rate of 1.5 ml/min and eluents were monitored at 225 nm.Results: The retention time of β-acetyldigoxin was 9.2 min. The method was found to be linear (R2= 0.9995) in the range of 31.25-500 µg/ml. The accuracy studies showed the mean percent recovery of 101.02%. LOD and LOQ were observed to be 0.289 µg/ml and 0.965 µg/ml, respectively. The method was found to be robust and system suitability testing was also performed. Forced degradation analysis was carried out under acidic, alkaline, oxidative and photolytic stress conditions. Significant degradation was observed under tested conditions, except for oxidative condition. The method was able to separate all the degradation products within runtime of 20 min and was able to determine β-acetyldigoxin unequivocally in presence of degradation products.Conclusion: The novel, economic, rapid and simple method for analysis of β-acetyldigoxin is reported. The developed method is suitable for routine quality control and its determination as API, and in pharmaceutical formulations and stability study samples.

scholarly journals Stability-indicating HPLC-DAD method for the determination of empagliflozin

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Shilpi Pathak ◽  
Pradeep Mishra
Keyword(s):  
Hplc Method ◽  
Coefficient Of Determination ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Validation Parameters ◽  
Forced Degradation Studies ◽  
Tablet Dosage

Abstract Background A stability-indicating RP-HPLC method was developed and validated for the estimation of empagliflozin drug and its tablet dosage form using a DAD detector. The mobile phase consisted of methanol/acetonitrile/0.1%OPA (75:20:5). The peak was observed at 2.54 min using 222.0 nm absorption maxima. Results Calibration curve plot was found within the range of 10–50 µg/mL. The coefficient of determination (R2) was found to be 0.9990. Forced degradation studies were performed for the empagliflozin in various conditions, and the results were calculated as %RSD values and were found to be within the limits. Conclusion The method was validated as per ICH guidelines with respect to all validation parameters.

DEVELOPMENT OF A VALIDATED STABILITY-INDICATING METHOD FOR ESTIMATION OF ETHIONAMIDE IN TABLETS BY RP-HPLC AND CHARACTERIZATION OF ITS ISOLATED ALKALI DEGRADATION PRODUCT

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (01) ◽  
pp. 20-27
Author(s):  
Sandeep S. Sonawane ◽  
◽  
Akshay S. Patil ◽  
Santosh S. Chhajed ◽  
Dimple S. Lalchandani ◽  
...  
Keyword(s):  
Degradation Product ◽  
Elevated Temperatures ◽  
Degradation Products ◽  
Hplc Method ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Rp Hplc ◽  
Photolytic Degradation ◽  
Alkali Hydrolysis

A simple, accurate, reproducible and specific stability-indicating RP-HPLC method was developed for estimation of ethionamide in tablets. Ethionamide was exposed to acid, alkali and neutral hydrolysis at elevated temperatures, to thermolytic degradation, peroxide-mediated oxidation at room temperature in dark and to photolytic degradation. The drug was found stable to thermolytic and photolytic conditions and to neutral hydrolysis. However, substantial degradation was obtained in acid and alkali hydrolysis and complete degradation in peroxide-medicated oxidation. Similar degradation behavior was observed when ethionamide tablets were exposed to the mentioned forced degradation conditions. The method showed adequate resolution of drug from its potential degradation products on C18 (250 × 4.6 mm, 5µ) column using mobile phase of methanol: water (50: 50 % V/V) at 1 mL/min. The drug and its potential degradation products were detected at 290 nm. The method was validated as per the ICH Q2(R1) guidelines. The enrichment of the alkali degradation product was performed and isolated by preparative TLC and further confirmed by NMR and IR spectroscopy.

scholarly journals Stability-Indicating RP-HPLC Method for Simultaneous Estimation of Enrofloxacin and Its Degradation Products in Tablet Dosage Forms

2015 ◽  
Vol 2015 ◽  
pp. 1-11 ◽  
Author(s):  
V. Ashok Chakravarthy ◽  
B. B. V. Sailaja ◽  
Avvaru Praveen Kumar
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Dosage Forms ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Column Temperature ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Tablet Dosage

The present work was the development of a simple, efficient, and reproducible stability-indicating reverse-phase high performance liquid chromatographic (RP-HPLC) method for simultaneous determination enrofloxacin (EFX) and its degradation products including ethylenediamine impurity, desfluoro impurity, ciprofloxacin impurity, chloro impurity, fluoroquinolonic acid impurity, and decarboxylated impurity in tablet dosage forms. The separation of EFX and its degradation products in tablets was carried out on Kromasil C-18(250×4.6 mm, 5 μm) column using 0.1% (v/v) TEA in 10 mM KH2PO4(pH 2.5) buffer and methanol by linear gradient program. Flow rate was 1.0 mL min−1with a column temperature of 35°C and detection wavelength was carried out at 278 nm and 254 nm. The forced degradation studies were performed on EFX tablets under acidic, basic, oxidation, thermal, humidity, and photolytic conditions. The degraded products were well resolved from the main active drug and also from known impurities within 65 minutes. The method was validated in terms of specificity, linearity, LOD, LOQ, accuracy, precision, and robustness as per ICH guidelines. The results obtained from the validation experiments prove that the developed method is a stability-indicating method and suitable for routine analysis.

scholarly journals Stability Indicating Simultaneous Validation of Telmisartan and Cilnidipine with Forced Degradation Behavior Study by RP-HPLC in Tablet Dosage Form

2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
Reema H. Rupareliya ◽  
Hitendra S. Joshi
Keyword(s):  
Correlation Coefficient ◽  
Degradation Products ◽  
Hplc Method ◽  
Array Detector ◽  
Forced Degradation ◽  
Solution Stability ◽  
Stability Indicating ◽  
Stress Studies ◽  
Rp Hplc ◽  
Behavior Study

A simple, precise, and accurate RP-HPLC method has been developed and validated for the simultaneous assay of Telmisartan and Cilnidipine in tablets. Isocratic RP-HPLC method was developed on Waters C18 250×4.6 mm, 5 μm column using mobile phase as acetonitrile (ACN): buffer pH 3.0 with orthophosphoric acid (68 : 32) at a flow rate of 1.0 mL/min and the detection was carried out at 245 nm using photodiode array detector. Forced degradation study was carried out by oxidation, hydrolysis, photolysis, and heating the drug. The method was validated for specificity, linearity, precision, accuracy, robustness, and solution stability. The method was found to be linear in the concentration range of 40–160 μg/mL with correlation coefficient of 0.9990 for Telmisartan and 10–40 μg/mL with correlation coefficient of 0.9989 for Cilnidipine. Degradation products produced as a result of stress studies did not interfere with the detection of agomelatine; therefore, the assay can be considered to be stability indicating.

A VALIDATED STABILITY INDICATING RP-HPLC METHOD FOR DETERMINATION OF AZELNIDIPINE AND ITS IMPURITIES IN PHARMACEUTICAL FORMULATION

INDIAN DRUGS ◽  
2020 ◽  
Vol 57 (08) ◽  
pp. 70-76
Author(s):  
Pavani Peddi ◽  
S. L. Tulasi ◽  
N. Usha Rani ◽  
T. Raja Rajeswari
Keyword(s):  
Degradation Products ◽  
Impurity Content ◽  
Hplc Method ◽  
Stability Study ◽  
Forced Degradation ◽  
Uv Detector ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Formulation Analysis

A novel simple, rapid, sensitive and stability-indicating RP-HPLC method was developed and validated for the determination of azelnidipine (ALDP) and its impurities 1 and 2. Resolution of drug, its potential impurities and degradation products were achieved by RP-HPLC on was performed on Prontosil ODS C18 column (250 mm x 4.6 mm, 5µ) using a mobile phase consisting of methanol and 0.1M sodium acetate 40: 60 (v/v) at a flow rate of 1 ml/min and 231 nm of UV detector. Validation of the method was performed along with formulation analysis and forced degradation studies. The calibration curves of ALDP were linear over a concentration range of 50-300 µg/mL. The method was rapid with a retention time of the impurity 2, impurity and ALDP observed at 3.60, 5.15 and 6.90 min, respectively. The method was applied for the impurities determination in drug tablets and for degradation products determination in a stability study of ALDP. The impurity content in the tablets was quantified as 0.1% of total drug. The method can also be used for rapid and accurate quantification of ALDP in its tablets during stability testing.

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