scholarly journals A Validated Stability-Indicating RP-HPLC Method for the Simultaneous Determination of Tenofovir, Emtricitabine, and a Efavirenz and Statistical Approach to Determine the Effect of Variables

2013 ◽  
Vol 2013 ◽  
pp. 1-8 ◽  
Author(s):  
Prashant S. Devrukhakar ◽  
Roshan Borkar ◽  
Nalini Shastri ◽  
K. V. Surendranath
Keyword(s):  
Degradation Products ◽  
Gradient Elution ◽  
Hplc Method ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Accelerated Stability ◽  
Successful Separation ◽  
Combined Drugs

A simple, rapid, and stability-indicating RP-HPLC method for a combination of tenofovir disoproxil fumarate (TDF), emtricitabine (FTC), and efavirenz (EFV) was developed and validated with the help of a suitable statistical software as an application tool for the quality by design. The drugs individually, and in combination, were subjected to forced degradation (thermal, photolytic, hydrolytic, and oxidative stress conditions) and accelerated stability studies (40 ± 1°C/75 ± 3% RH for three months). Successful separation of combined drugs from degradation products was achieved by gradient elution on a reverse-phase C18 column, using a mobile phase containing phosphate buffer (pH 3.5): acetonitrile at 1.5 mL min−1 flow rate, detection wavelength 256 nm, column oven temperature 25°C, and injection volume 10 μL. Linearity was established in the range of 20–300 μg mL−1, 24.5–367.5 μg mL−1 and 60–900 μg mL−1 for FTC, TDF, and EFV, respectively. The method was successfully applied for quantifying the drugs in marketed dosage forms and on stability samples.

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.

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.

scholarly journals DEVELOPMENT AND VALIDATION OF A STABILITY INDICATING RP-HPLC METHOD FOR THE DETERMINATION OF POTENTIAL DEGRADATION PRODUCTS OF DIFLUPREDNATE IN OPHTHALMIC EMULSION

2018 ◽  
Vol 10 (9) ◽  
pp. 79 ◽  
Author(s):  
Murlidhar V. Zope ◽  
Rahul M. Patel ◽  
Ashwinikumari Patel ◽  
Samir G. Patel
Keyword(s):  
Quantitative Determination ◽  
Degradation Product ◽  
Mobile Phase ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Hplc Method ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Rp Hplc

Objective: The objective of the current study was to develop and validate a simple, robust, precise and accurate RP-HPLC (reverse phase-high performance liquid chromatography) method for the quantitative determination of potential degradation products of Difluprednate (DIFL) in the ophthalmic emulsion.Methods: Chromatographic separation was achieved on the YMC pack ODS-AQ (150× 4.6) mm, 3μm column with a mobile phase containing a gradient mixture of mobile phase A (0.02M Ammonium formate buffer pH 4.5 adjusted with formic acid) and Acetonitrile as mobile phase B, at flow rate of 1.5 ml/min and with UV detection at 240 nm.Results: The peak retention time of DIFL was found at about 17.2 min, the RRT of degradation product-1 (DP-1), degradation product-2 (DP-2), and degradation product-3 (DP-3), were found to be about 0.49, 0.65 and 0.79 respectively (calculated with respect to Difluprednate). Stress testing was performed in accordance with an ICH (international council for harmonisation) guideline Q1A (R2) [1]. The method was validated as per ICH guideline Q2 (R1)[2]. The calibration curve was found to be linear in the concentration range of 0.1 to 0.75 µg/ml for Difluprednate, DP-1, DP-2 and DP-3. The LOD (Limit of detection) was found to be 0.1µg/ml and LOQ (Limit of quantification) of 0.15µg/ml for Difluprednate, DP-1, DP-2 and DP-3 respectively. The recovery from LOQ to 150% was within 90-110%. The forced degradation data confirms the stability indicating the nature of the method.Conclusion: A simple, robust, precise and accurate RP-HPLC method for the quantitative determination of potential degradation products of Difluprednate in the ophthalmic emulsion was developed and validated. 

scholarly journals A Rapid Stability-Indicating RP-HPLC Method for the Determination of Betaxolol Hydrochloride in Pharmaceutical Tablets

2013 ◽  
Vol 8 ◽  
pp. ACI.S11256 ◽  
Author(s):  
Sylvain Auvity ◽  
Fouad Chiadmi ◽  
Salvatore Cisternino ◽  
Jean-Eudes Fontan ◽  
Joël Schlatter
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Potassium Dihydrogen Phosphate ◽  
Reversed Phase ◽  
Hplc Method ◽  
Forced Degradation ◽  
Dihydrogen Phosphate ◽  
Stability Indicating ◽  
Rp Hplc

A stability-indicating reversed-phase high performance liquid chromatography (RP-HPLC) method was developed for the determination of betaxolol hydrochloride, a drug used in the treatment of hypertension and glaucoma. The desired chromatographic separation was achieved on a Nucleosil C18, 4 μm (150 × 4.6 mm) column, using isocratic elution at a 220 nm detector wavelength. The optimized mobile phase consisted of a 0.02 M potassium dihydrogen phosphate: methanol (40:60, v/v, pH 3.0 adjusted with o-phosphoric acid) as solvent. The flow rate was 1.6 mL/min and the retention time of betaxolol hydrochloride was 1.72 min. The linearity for betaxolol hydrochloride was in the range of 25 to 200 μg/mL. Recovery for betaxolol hydrochloride was calculated as 100.01%-101.35%. The stability-indicating capability was established by forced degradation experiments and the separation of unknown degradation products. The developed RP-HPLC method was validated according to the International Conference on Harmonization (ICH) guidelines. This validated method was applied for the estimation of betaxolol hydrochloride in commercially available tablets.

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 STABILITY INDICATING HPLC METHOD FOR DETERMINATION OF VILAZODONE HYDROCHLORIDE

2017 ◽  
Vol 9 (4) ◽  
pp. 123
Author(s):  
Birva A. Athavia ◽  
Zarna R. Dedania ◽  
Ronak R. Dedania ◽  
S. M. Vijayendra Swamy ◽  
Chetana B. Prajapati
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Hplc Method ◽  
Alkaline Condition ◽  
Forced Degradation ◽  
Molecular Formula ◽  
Stability Indicating ◽  
Dry Heat ◽  
Limit Of Quantitation

Objective: The aim and objective of this study was to develop and validate Stability Indicating HPLC method for determination of Vilazodone Hydrochloride.Methods: The method was carried out on a Phenomenex, C18 (250x4.6 mm, 5 µm) Column using a mixture of Acetonitrile: Water (50:50v/v), pH adjusted to 3.3 with Glacial Acetic Acid for separation. The flow rate was adjusted at 1 ml/min and Detection was carried out at 240 nm.Results: The retention time of vilazodone hydrochloride was found to be 2.3 min. The calibration curve was found to be linear in the range 25-75µg/ml with a correlation coefficient (R2=0.996). The limit of detection and limit of quantitation were found to be 4.78µg/ml and 14.48µg/ml respectively. The % recovery of vilazodone hydrochloride was found to be in the range of 98.21±0.08 % to 99.07±0.64%. The proposed method was successfully applied for the estimation of vilazodone hydrochloride in marketed tablet formulation.Vilazodone Hydrochloride was subjected to forced degradation under Acidic, Alkaline, Oxidation, Dry Heat and Photolytic degradation conditions. Vilazodone hydrochloride showed 3.12% degradation under acidic condition, 4.78% under alkaline condition, 7.8% under oxidation condition, 3.53% under dry heat condition and 4.9% under photolytic condition.Acid degradation impurity was identified and characterised by LC-MS/MS was found to be 1-(4-Penten-1-yl) piperazine having molecular weight 154.253 (m/z 155.08) and Molecular Formula C9H18N2.Conclusion: A simple, precise, rapid and accurate Stability Indicating HPLC method has been developed and validated for the determination of Vilazodone Hydrochloride in presence of its degradation products as per the ICH Guidelines. 

scholarly journals Stability Indicating RP-HPLC Method for Determination of Valsartan in Pure and Pharmaceutical Formulation

2010 ◽  
Vol 7 (1) ◽  
pp. 246-252 ◽  
Author(s):  
S. K. Patro ◽  
S. K. Kanungo ◽  
V. J. Patro ◽  
N. S. K. Choudhury
Keyword(s):  
Linear Response ◽  
Mobile Phase ◽  
Hplc Method ◽  
Forced Degradation ◽  
Control Analysis ◽  
Solution Stability ◽  
Stability Indicating ◽  
Quality Control Analysis ◽  
Rp Hplc

A simple, rapid and accurate and stability indicating RP-HPLC method was developed for the determination of valsartan in pure and tablet forms. The method showed a linear response for concentrations in the range of 50-175 µg/mL using 0.01 M NH4H2PO4(pH 3.5) buffer: methanol [50:50] as the mobile phase with detection at 210 nm and a flow rate of 1 mL/min and retention time 11.041 min. The method was statistically validated for accuracy, precision, linearity, ruggedness, robustness, forced degradation, solution stability and selectivity. Quantitative and recovery studies of the dosage form were also carried out and analyzed; the % RSD from recovery studies was found to be less than 1. Due to simplicity, rapidity and accuracy of the method, we believe that the method will be useful for routine quality control analysis.

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.

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