scholarly journals Stability Indicating RP-HPLC Method for Estimation of Fexofenadine Hydrochloride in Pharmaceutical Formulation

2012 ◽  
Vol 9 (3) ◽  
pp. 1257-1265 ◽  
Author(s):  
H. M. Nimje ◽  
Shital T. Nimje ◽  
R. J. Oswal ◽  
S. T. Bhamre
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Parent Compound ◽  
Hplc Method ◽  
Uv Detector ◽  
Oxidation Condition ◽  
Stability Indicating ◽  
Stress Studies ◽  
Tablet Dosage

A stability-indicating HPLC method was developed and validated for the quantitative determination of fexofenadine in tablet dosage forms. An isocratic seperation was achieved using a Zorbax, Eclipse XBD, C-8 Column having 150 x 4.6 mm i.d., 5 µm particle size column with flow rate of 1.2 ml/min and using UV detector to monitor the eluate at 210 nm. The mobile phase consist of phosphate buffer: acetonitrile: methanol (60:20:20; v/v/v) with pH 3.7 adjusted with o-phosphoric acid. The drug was subjected to oxidation, hydrolysis, photolysis and thermal degradation. Fexofenadine was found to degrate in acidic, basic and oxidation condition. Complete seperation of degraded product was achieved from parent compound. All degradation products in an overall analytical run time of approximately 60 min with the parent compound fexofenadine eluting at approximately 12.1 ±0.9 min. The method was linear over the concentration range of 1-100 µg/ml (r2= 0.9970) with limit of detection and quatification of 0.2 µg/ml and 0.6 µg/ml, respectively. The method has the requisite accuracy, selectivity, sencitivity, precision and robustness to assay fexofenadine in tablets. Degradation products resulting from stress studies did not interfere with the detection of fexofenadine and the assay is thus stability indicating.

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. 

A new stability indicating chiral RP-HPLC method for determination of degradation products in Meclizine Hydrochloride

2020 ◽  
Vol 16 ◽  
Author(s):  
Bryan Gowramma ◽  
Ramachandran Senthil Kumar ◽  
Kaviarasan Lakshmanan ◽  
Rajagopal Kalirajan ◽  
Subramanian Nainar Meyyanathan
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Pharmaceutical Preparations ◽  
Hplc Method ◽  
Stress Conditions ◽  
Main Peak ◽  
Uv Detector ◽  
Limit Of Quantification ◽  
Degradation Behaviour ◽  
Stability Indicating

Background: An enantiomeric separation of stability-indicating high-performance liquid chromatographic method was developed and validated for the analysis of Meclizine enantiomers. The degradation behaviour of Meclizine Hydrochloride was investigated under different stress conditions recommended by International Conference on Harmonization (ICH). Experiment: Enantiomeric resolution of the drug and complete separation from its degradation products were successfully achieved on a Phenomenex® lux cellulose 1 C18 (250 mm × 4.6 mm i.d, 5 µm particle size) column, using UV detector at a wavelength of 230 nm, with mobile phase consisting of acetonitrile, 20mM ammonium bicarbonate at the ratio of 75:25 (v/v), and a flow rate of 1 mL/min. The drug was subjected to alkaline, acidic, neutral, oxidative and photolytic conditions in order to mimic stress conditions. Result: The degradation products were well resolved from main peak and proving the stability-indicating power of the method. The developed method provided linear responses within the concentration range 1-5 µg/mL, and regression analysis showed a correlation coefficient value (r2) of 0.999. The HPLC method was validated as per ICH guidelines with respect to specificity, precision, linearity and robustness. Limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.25 µg/mL and 1.00 µg/mL respectively. Conclusion: The method provides good sensitivity and excellent precision and reproducibility. The method was highly selective, where degradation products and co formulated compounds did not interfere. The proposed method was successfully applied in pharmaceutical preparations.

STABILITY INDICATING HPLC-MS/UV METHOD FOR DETERMINATION OF RACECADOTRIL FROM BULK AND FORMULATION

INDIAN DRUGS ◽  
2016 ◽  
Vol 53 (12) ◽  
pp. 25-30
Author(s):  
V. S Tambe ◽  
◽  
M. N. Deodhar ◽  
V. Prakya
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Degradation Products ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Ionization Mass ◽  
Capsule Formulation ◽  
Stability Indicating ◽  
Positive Mode

The present work was focused on the development of rapid, specific and novel stability indicating high performance liquid chromatographic method for determination of racecadotril (RAC) in bulk and capsule formulation. The drug and formulation were subjected to hydrolysis (acidic, alkaline and neutral), oxidative and thermal stress, as per ICH guidelines Q1A (R2). Degradation products of RAC formed under various stress conditions were well separated using a mobile phase containing acetonitrile and water (60:40 V/V) with 0.5% formic acid. Quantification was performed using RP C18 column with the detection wavelength of 230 nm.The method was considered linear in the concentration range of 5-100 μg mL−1 for RAC. Limit of detection and quantitation was found to be 0.15 and 0.45 μg mL−1 respectively. Identification of major stress degradation products was performed using qudrupole electrospray ionization mass spectroscopy (ESI-MS) in positive mode. RAC was found to be very unstable under basic condition and is converted into 2-(3-(acetylthio)-2-benzylpropanamido) acetic acid and 2-benzyl-N-(2-hydroxyvinyl) acrylamide. The drug is more stable at neutral pH as compared to acidic and oxidative stress. Under acidic conditions, benzyl 2-(2-benzyl-3-mercaptopropanamido) acetate is the probable degradation product. A stability indicating HPLC method was developed for quantitation of RAC. A strict control should be exerted on the level of basic impurities in formulations.

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 A SIMPLE (HPLC–UV) METHOD FOR THE QUANTIFICATION OF COLCHICINE IN BULK AND ETHOSOMAL GEL NANO-FORMULATION AND ITS VALIDATION

2017 ◽  
Vol 9 (7) ◽  
pp. 72 ◽  
Author(s):  
Ibrahim M. Abdulbaqi ◽  
Yusrida Darwis ◽  
Nurzalina Abdul Karim Khan ◽  
Reem Abou Assi ◽  
Gabriel Onn Kit Loh
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Reversed Phase ◽  
Hplc Method ◽  
Acid Oxidation ◽  
Limit Of Quantification ◽  
Stability Indicating ◽  
Stress Degradation

Objective: To develop and validate a stability-indicating reversed phase high-performance liquid chromatography (RP-HPLC) method for the determination of colchicine in bulk and ethosomal gel nano-formulation.Methods: The chromatographic conditions were optimized using stainless steel Hypersil Gold C-18 analytical column with the dimensions of 250 mm x 4.6 mm ID x 5 µm. The mobile phase consisted of acetonitrile and ammonium acetate buffer (20 mmol/l, pH=4.85) in the ratio of 32:68 v/v. The flow rate was set at 1 ml/min and the detection wavelength was 353 nm. The column was maintained at 30 °C and the injection volume was 10 µl. The stability of colchicine in different conditions was investigated by exposing the drug to stress degradation using acid, base, oxidation, heat and light.Results: There was no interference from excipients, impurities, dissolution media or degradation products at the retention time of colchicine 5.9 min indicating the specificity of the method. The limit of detection (LOD) and the limit of quantification (LOQ) were 8.64 ng/ml and 26.17 ng/ml respectively. The drug showed good stability under heat, acid, oxidation and light, but substantial degradation was observed under alkali condition. The procedure was validated for specificity, linearity, accuracy and precision.Conclusion: A simple, rapid, specific and stability-indicating HPLC–UV method for the determination of colchicine in the pure and ethosomal gel was successfully developed. The developed method was statistically confirmed to be accurate, precise, and reproducible.

Stability indicating RP-HPLC method for the determination of Tenofovir in pharmaceutical formulation

2021 ◽  
pp. 6335-6339
Author(s):  
Gurmeet S. Chhabra ◽  
Aayushi Rajora ◽  
Dinesh K. Mishra
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Pharmaceutical Products ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Stability Indicating ◽  
Stress Studies ◽  
Ich Guidelines ◽  
Solid Dose

Stability indicating high performance liquid chromatography (HPLC) method was developed for the assay of Tenofovir in bulk and solid dose formulation. The HPLC separation was achieved on kromasil C18 (100mm × 4.6mm, 5 μm) column using a mobile phase of Methanol: Potassium dihydrogen orthophosphate buffer (30:70,v/v) at a flow rate of 1 ml min-1 and UV detection at 260 nm. Peak elutes at 7.33 appropriate. The method was validated for linearity, repeatability, accuracy, precision, robustness, limit of detection and limit of quantification. The accuracy was between 99.14 - 99.97%. The highest R.S.D. amongst interday and Intraday precision was found 0.808 and 0.473 respectively.The assay was linear over the concentration range of 10-50 μg/ml (R≈0. 999). The method was robust as no significant change in chromatographic parameters. LOD and LOQ was found to be 0.90 and 2.71 respectively. The stress studies were performed per ICH guidelines to confirm its Stress testing was carried out in presence of acid, base, hydrogen peroxide, heat and light to demonstrate specificity of the method as per ICH guidelines. The developed method could separate the potential degradation products from the Tenofovir peak. It was concluded that highest degradation occurs in basic condition. This proposed method was suitable and practical for analysis the content of Tenofovir in pharmaceutical products and could be of benefit for the prediction shelf life of Tenofovir in marketed formulations.

scholarly journals Development and validation of Stability Indicating HPLC method for determination of Ellagic and Gallic acid in Jambul seed

2015 ◽  
Vol 3 (3) ◽  
pp. 434-438 ◽  
Author(s):  
Mrinalini Damle ◽  
Nilam Dalavi
Keyword(s):  
Gallic Acid ◽  
Ellagic Acid ◽  
Limit Of Detection ◽  
Ethanolic Extract ◽  
Hplc Method ◽  
Uv Detector ◽  
Stability Indicating ◽  
Stress Degradation ◽  
Development And Validation

Ellagic and Gallic acid are main phytoconstituents of S.cumini seeds. These are the phenolic compounds. An approach for the stress degradation was successfully applied for the development of stability indicating HPLC method for the determination of Ellagic and Gallic acid. Sample was resolved on a Hypersil C18 (250*4.6 mm particle size 5?) column. The mobile phase consisted of 1% OPA and ACN and in the ratio of 70:30 v/v which was sonicated to degas and delivered at a flow rate of 1ml/min at ambient temperature. The retention time of Ellagic acid and Gallic acid was 3.1±0.05 & 4.1±0.05 minutes. Studies were performed using an HPLC system equipped with a UV detector; the response was monitored at 271nm. The method is specific to Ellagic and Gallic acid; it is able to resolve the peak from ethanolic extract of s.cumini seeds and formulation. The calibration curve was linear over the concentration range of 8-24 ?g/ml (r2=0.997, 0.998 resp). The limit of detection for  Ellagic acid and Gallic acid   was found to be 0.25?g/ml, 0.15?g/ml resp. and the quantification limit was about 0.75?g/m, 0.49?g/ml. The accuracy of the method was established based on the recovery studies. The markers were subjected to acid, base, neutral hydrolysis, oxidation, thermal degradation and photolysis. The method was successfully validated according to ICH guidelines Q2 (R1).Int J Appl Sci Biotechnol, Vol 3(3): 434-438

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 Validated RP-HPLC Method and Force Degradation Studies of Fexofenadine Hydrochloride in Pharmaceutical Dosage Form

2018 ◽  
Vol 17 (1) ◽  
pp. 43-50
Author(s):  
Sherejad Sanam ◽  
Sharmin Nahar ◽  
Nazmus Saqueeb ◽  
SM Abdur Rahman
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Parent Compound ◽  
Hplc Method ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Fexofenadine Hcl

A stability indicating HPLC method was developed and validated for the quantitative determination of fexofenadine hydrochloride. An isocratic separation was achieved using phenomenex (C18) column (250×4.6 mm, 5 μm) with flow rate of 1.0 ml/min and UV detection at 254 nm. The mobile phase consists of 5Mm acetate buffer: acetonitrile (50:50; v/v) with pH 9.4 adjusted with acetic acid. The drug was subjected to oxidative, acidic, basic, neutral, photolytic and thermal degradation. All degradation products were eluted in an overall analytical run time of approximately 40 min with the parent compound fexofenadine hydrochloride at a flow rate of approximately 3.3±0.3 min. The method was linear over the concentration range of 31.5-500 μg/ml (r2 = 0.999) with limit of detection and quantification of 3.5 μg/ml and 10.1 μg/ml, respectively. The method has the requisite accuracy, selective, precision and robustness to assay fexofenadine HCl in tablets.Dhaka Univ. J. Pharm. Sci. 17(1): 43-50, 2018 (June)

scholarly journals Monitoring of the photochemical stability of carvedilol and its degradation products by the RP-HPLC method

2007 ◽  
Vol 72 (1) ◽  
pp. 37-44 ◽  
Author(s):  
Jelena Stojanovic ◽  
Sote Vladimirov ◽  
Valentina Marinkovic ◽  
Dragan Velickovic ◽  
Predrag Sibinovic
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Uv Detector ◽  
Stability Indicating ◽  
Liquid Chromatographic Method ◽  
Bulk Drug ◽  
Liquid Chromatographic

A sensitive, selective, precise and stability-indicating, new high-performance liquid chromatographic method for the analysis of carvedilol both as a bulk drug and in formulations was developed and validated. As the method could effectively separate the drug from its degradation products, it can be employed as a stability-indicating one. The method was validated for linearity, selectivity, precision, robustness, LOD, LOQ and accuracy. The chromatographic separation was achieved on a Chromolit RP8e, 100x4.6 mm, analytical column. The mobile phase consisted of a mixture of acetonitrile and water (45:55, V/V) (pH 2.5), pH adjusted with formic acid. The absorbance was monitored with a UV detector at 280 nm and the temperature of the analyses was 40?C. The flow rate was 0.5 mL/min. The linearity (r? 0.999), reproducibility (0.68-1.27 %) and recovery (99.71-101.58) were found to be satisfactory. This method enables the simultaneous determination of carvedilol and its degradation products, as well as stability. .

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