scholarly journals Forced Degradation Study for Simultaneous Quantification of Aspirin and Omeprazole in Pharmaceutical Dosage form by RP-HPLC

2021 ◽  
pp. 143-150
Author(s):  
Chandni Chandarana ◽  
Pankaj Kapupara ◽  
Parixit Prajapati
Keyword(s):  
Thermal Degradation ◽  
Oxidative Degradation ◽  
Hplc Method ◽  
Forced Degradation ◽  
Pharmaceutical Dosage Form ◽  
Degradation Study ◽  
Pharmaceutical Ingredients ◽  
Rp Hplc ◽  
Acid And Base ◽  
Hydrolysis Conditions

Aims: To study force degradation of aspirin and omeprazole simultaneously by RP-HPLC method Study design: RP-HPLC method was used to measure % degradation. Place and Duration of Study: Study was carried out at center of excellence, G.I.D.C., vapi-396195, Gujarat, India between June 2019 to march 2020. Methodology: A force degradation study of aspirin and omeprazole was carried out simultaneously. The drugs were subjected to various degradation conditions like hydrolysis by acid and base, Oxidative degradation, and thermal degradation study. Results: For acidic condition, the degradation was found to be 32.63 % for aspirin and 61.64 % for omeprazole. For basic condition, the degradation was found to be 10.17 % for aspirin and 4.29 % for omeprazole. By oxidative hydrolysis, the aspirin was degraded by 15.48 % and omeprazole was degraded by 26.38 %. By thermal degradation, 0.37 % degradation was observed for aspirin and 4.32 % degradation for omeprazole. Conclusion: In this proposed method the retention time for drug is less than 8 min, which is less then available method. For omeprazole, strong degradation was observed in acidic conditions and mild in basic hydrolysis conditions. For aspirin, more degradation was observed in basic conditions than acidic hydrolysis. Both drugs were degraded in oxidative conditions using 3% H2O2. Omeprazole degraded more than aspirin by dry heat degradation. The method was successfully applied for the quantitative determination of both Active Pharmaceutical Ingredients.

FORCED DEGRADATION STUDIES OF TIZANIDINE HYDROCHLORIDE AND DEVELOPMENT OF VALIDATED STABILITY-INDICATING RP-HPLC METHOD

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (4) ◽  
pp. 50-55
Author(s):  
Shahbaz Rathor ◽  
Atul Sherje ◽  
Keyword(s):  
Thermal Degradation ◽  
Hplc Method ◽  
Base Hydrolysis ◽  
Forced Degradation ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Stress Studies ◽  
Stability Indicating Method ◽  
Rp Hplc ◽  
Forced Degradation Studies

Simple and precise stability indicating RP-HPLC method for the quantitative determination of tizanidinehydrochloride (TZN) in pharmaceutical dosage form was developed and validated. The separation was achieved using Atlantis C18 column (250 x 4.6 mm, 5µm) at 25 °C using a mobile phase containing 20mM KH2 PO4 (pH 3.5):methanol in the ratio of 30:70 V/V at 0.8 mL/min flow rate and 315nm detection wavelength. The retention time for TZN was 3.7 min and showed linearity in the 5-40µg/mL range with R2 >0.99. The drug was subjected to acid/ base hydrolysis, oxidative and thermal degradation to establish stability indicating method. The method was validated as per ICHQ2 (R1) guidelines. The method was accurate, precise, and specific for TZN estimation. In stress studies, the drug was found to be stable to acid/alkaline hydrolysis, oxidation, and thermal degradation conditions. Thus, the reported method can be used as a stability-indicating method for quality control and routine analysis of TZN.

scholarly journals Development, Validation and Forced Degradation Study of Emtricitabine and Tenofovir Alafenamide in its Pharmaceutical Dosage Form Using RP-HPLC

2021 ◽  
pp. 37-46
Author(s):  
Khushboo Patel ◽  
Ujashkumar Shah ◽  
Hirak Joshi ◽  
Jayvadan K. Patel ◽  
Tejas B. Patel
Keyword(s):  
Mobile Phase ◽  
Limit Of Detection ◽  
Solvent System ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Pharmaceutical Dosage Form ◽  
Degradation Study ◽  
Rp Hplc ◽  
Tenofovir Alafenamide

Aims: The present research was aimed to develop and validate a reverse phase high performance liquid chromatographic (RP-HPLC) method for the quantification of Emtricitabine (EMT) and Tenofovir Alafenamide (TEN) in combination. Methodology: Separation was achieved under optimized chromatographic condition on an Inertsil C18, 250 x 4.6 mm, 5μm column. Various composition of mobile phase was tried. Separation of EMT and TEN was started with Methanol: Buffer and Methanol finally using solvent system of Buffer (pH 3.5) and Methanol in ratio of (30:70) and flow rate adjust at 1.0 ml/min was used as solvent system, the detection was carried out at 262nm using Shimazdu UV-visible detector. The mobile phase run time for the developed analytical method was 10 minutes. Results: The standard curve was found linear in the concentration range of 20-60 μg/ ml (r2- 0.9994) and 2.5-7.5 μg/ ml (r2-0.9992) for EMT and TEN respectively. The %RSD was found to be 0.80-0.95% and 0.63-1.09 for EMT and TEN respectively. Percentage (%) recoveries for EMT and TEN to be in range of 100%-100.6% and 99.32%-100.83% respectively. The limit of detection and the limit of quantification were found to be 4.80 μg/ ml and 14.7 μg/ ml respectively for EMT and 0.11 μg/ ml and 0.33μg/ ml respectively for TEN. Results of forced degradation study showed EMT degradation in acid and base medium while TEN was showed degradation in oxidative stress. The proposed developed RP-HPLC method was validated statistically and the values were found to be within the acceptable limits. Conclusion: In conclusion, the developed RP-HPLC method was found to be simple, specific, and rugged for simultaneous estimation of EMT and TEN. Validation results of method was found within the acceptable limits. Hence it can be used for analysis of EMT and TEN.

scholarly journals A novel RP- HPLC method development and forced degradation studies for semaglutide in active pharmaceutical ingredients and pharmaceutical dosage form

2019 ◽  
Vol 10 (2) ◽  
pp. 865-873
Author(s):  
Arun Kumar Kuna ◽  
Ganapathi S ◽  
Radha GV
Keyword(s):  
Method Development ◽  
Active Pharmaceutical Ingredient ◽  
Hplc Method ◽  
Forced Degradation ◽  
Simple Method ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Ingredients ◽  
Rp Hplc ◽  
Forced Degradation Studies ◽  
Hplc Method Development

This research objective is for the development of a specific and simple method to trace Semaglutide presence in active pharmaceutical ingredient and pharmaceutical dosages. As part of a study on Semaglutide drug, solvents of HPLC grade waters HPLC instrument (Empower software) with PDA detector, ultrasonicator (Make: Labman) and pH meter (Make: Adwa) are used. The Method was optimized with mobile phase with a composition of buffer and solvent were of 60:40%v/v, flow maintained was 1.0ml/min, the injection volume of 10µl, run time was 5min. All separations were performed with PDA detector and column used was Discovery C18 150 x 4.6mm, 5m. Results for the developed method are accurate and specific. The detection wavelength was 292 nm, the retention time for Semaglutide was 2.689min, linearity resulted with r2= 0.9998, % RSD for precision was 1.0; %mean recovery for accuracy was in the range of 99.73 to 100.29.  This study report is for industrial application for determining Semaglutide presence in pharmaceutical ingredient and dosages.

scholarly journals SIMULTANEOUS ESTIMATION, VALIDATION, AND FORCED DEGRADATION STUDIES OF BETAHISTINE DIHYDROCHLORIDE AND DOMPERIDONE IN A PHARMACEUTICAL DOSAGE FORM USING RP-HPLC METHOD

2018 ◽  
Vol 11 (10) ◽  
pp. 125
Author(s):  
Vaishali Mistry ◽  
Rohan Mishra
Keyword(s):  
Hplc Method ◽  
Base Hydrolysis ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Uv Detector ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Betahistine Dihydrochloride ◽  
The Stability

Objective: This study describes the stability-indicating reverse-phase high-performance liquid chromatography (RP-HPLC) method for simultaneous estimation of betahistine dihydrochloride and domperidone in pharmaceutical dosage forms.Methods: The proposed RP-HPLC method was developed using Shimadzu Prominence-i LC-2030 HPLC system equipped with UV detector and chromatographic operation was carried on Shim-pack C18 (250 mm×4.6 mm, 5 μ) column at a flow rate of 1 ml/min and the run time was 10 min. The mobile phase consisted of methanol and water in the ratio of 80:20% v/v and eluents were scanned using a UV detector at 244 nm.Results: The retention time of betahistine dihydrochloride and domperidone was found to be 2.3 and 3.6 min, respectively. A linearity response was observed in the concentration range of 9.6 μg/ml–22.4 μg/ml for betahistine dihydrochloride and 6–14 μg/ml for domperidone, respectively. Limit of detection and limit of quantification for betahistine dihydrochloride were 0.52 μg/ml and 1.58 μg/ml and for domperidone are 0.64 μg/ml and 1.94 μg/ml, respectively.Conclusion: The stability-indicating method was developed by subjecting drugs to stress conditions such as acid and base hydrolysis, oxidation, photo and thermal degradation, and degraded products formed were resolved successfully from samples.

scholarly journals METHOD DEVELOPMENT AND VALIDATION FOR THE ESTIMATION OF ENTECAVIR IN BULK AND PHARMACEUTICAL DOSAGE FORMS BY RP-HPLC

2017 ◽  
pp. 107-111
Author(s):  
Swathi P. ◽  
S. Vidyadhara ◽  
R. L. C. Sasidhar ◽  
K. Kalyan Chakravarthi
Keyword(s):  
Flow Rate ◽  
Dosage Forms ◽  
Hplc Method ◽  
Forced Degradation ◽  
Uv Detector ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Validation Parameters ◽  
Degradation Studies

Objective: The objective and purpose of the analysis have sensibly assessed by selecting of a rapid and sensitive RP-HPLC method for Entecavir in bulk and pharmaceutical dosage form by using the most commonly employed C-18column with UV detection.Methods: In estimation by RP-HPLC method Agilent 1120 compact LC system with variable programmable UV detector and Rheodyne injector with 20 µl fixed loop was used for the chromatographic separation. The mode of operation was isocratic with the components of a solution consisting of methanol: acetonitrile(70:30v/v) and triethanolamine (2-4drops)at the flow rate of 1.2 ml/min and run time was 10 min. Forced degradation studies were conducted to evaluate the stability and specificity of the method along with the validation parameters.Results: Validation parameters of HPLC were found at a detection wavelength of 255 nm. Linearity was observed with the concentration range (Beer’s law range) 20-100µg/ml with R2=0.9991. Robustness with detection wavelengths 253 and 257 nm with a flow rate of 1 ml/min and 1.4 ml/min showed good results. The retention time of the drug was 2.64 min and assay showed 98.1%.Conclusion: The proposed RP-HPLC method was validated as per the ICH Q2B Guidelines, and was found to be applicable for routine quantitative analysis of Entecavir by RP-HPLC using UV detector in pharmaceutical dosage forms. The results of linearity, precision, accuracy and specificity, were proved, that does not exceed certain specified limits. The method provides selective quantification with no interference from other formulation excipients. The proposed method was highly sensitive, reproducible, reliable, robust and specific. Therefore, this method is a simple, rapid analysis may actually be more desirable than a more complicated and time-consuming process. The degradation studies at various stress conditions like thermal and hydrolytic, drug gets degraded at a temperature of 80 °c and refluxing with water at 70 °c for 24hours. 

HPLC METHOD DEVELOPMENT, VALIDATION, AND FORCED DEGRADATION FOR SIMULTANEOUS ANALYSIS OF OXYCODONE AND NALTREXONEIN PHARMACEUTICAL DOSAGE FORM

INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (02) ◽  
pp. 31-38
Author(s):  
R. S. Ch Phani ◽  
◽  
K. R. S. Prasad ◽  
R. M Useni
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Hplc Method ◽  
Forced Degradation ◽  
Solution Stability ◽  
Pharmaceutical Dosage Form ◽  
Column Temperature ◽  
Degradation Study ◽  
Ich Guidelines ◽  
Hplc Method Development

A simple, precise and stability-indicating RP-HPLC method was developed for simultaneous quantification of oxycodone (OXCD) and naltrexone (NTRX) in combined dosage form. The developed method was validated with respect to precision, linearity, accuracy, robustness, ruggedness, sensitivity and solution stability. The method was developed with ammonium di hydrogen phosphate buffer (pH 5.0) and acetonitrile in a ratio of 55:45 (v/v) as mobile phase at a flow rate of 1.0 mL/minute over Intersil ODS C18 column (250 mm × 4.6 mm×5μ).The UV detection wavelength was fixed at 235 nm. The column temperature was maintained at ambient temperature. The method showed good linearity with correlation coefficient values of 0.9990 and 0.9994 for OXCD and NTRX. The percent recoveries of the two drugs found within the limits of 98.0–102.0%. The LOQ concentrations of OXCD and NTRX are 0.625 μg/ mL and 0.075 μg/mL, respectively. The LOD concentrations of OXCD and NTRX are 0.3125 μg/mL and 0.0375 μg/mL, respectively. According to ICH guidelines forced degradation study was validated.

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 Validation of Stability Indicating Method and Degradation Kinetic Study of Apremilast

2020 ◽  
Vol 10 (2) ◽  
pp. 76-85
Author(s):  
Jitesha Patel ◽  
Parin Chokshi ◽  
Rajashree Mashru
Keyword(s):  
Kinetic Study ◽  
Hplc Method ◽  
Forced Degradation ◽  
Order Kinetic ◽  
Degradation Kinetic ◽  
Degradation Study ◽  
Potassium Dihydrogen ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Rp Hplc

A novel stability indicating RP- HPLC method was developed for the estimation of Apremilast in bulk and marketed formulation. Separation was achieved by using Shimadzu HPLC Analytical Technologies Limited C18 (250 mm x 4.6 mm, 5µm) as stationary phase. The optimized mobile phase consist of potassium dihydrogen ortho phosphate (pH-3.2): acetonitrile in ratio of 40:60 %v/v with flow rate of 1mL/min by using methanol as diluent. Retention time of Apremilast was found to be 5.4 min which was estimated at wavelength 360nm. Linearity of Apremilast was observed in the concentration range of 50-400µg/mL with r² value of 0.9999. Assay of Apremilast tablet was found to be 99.14-100.75%. Stability indicating nature of RP- HPLC method was estimated by conducting degradation kinetic study. The forced degradation of Apremilast bulk indicate that degradation in acidic, alkali, oxidative and photolysis condition were found to be 21%, 6.5%, 25.7% and 3.9% respectively. The kinetic study of apremilast in alkali degradation followed first order kinetic study. The result indicate that the developed RP-HPLC method is suitable for estimation of Apremilast in presence of degradant product. The above method was validated as per ICH guideline. Keywords: Apremilast, RP-HPLC, Validation, Forced Degradation Study, Alkali Degradation Kinetic study

scholarly journals Stability-Indicating Validated Novel RP-HPLC Method for Simultaneous Estimation of Methylparaben, Ketoconazole, and Mometasone Furoate in Topical Pharmaceutical Dosage Formulation

2013 ◽  
Vol 2013 ◽  
pp. 1-9 ◽  
Author(s):  
Chinmoy Roy ◽  
Jitamanyu Chakrabarty
Keyword(s):  
Limit Of Detection ◽  
Hplc Method ◽  
Mometasone Furoate ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Solution Stability ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Dosage Formulation

A simple, specific, precise, and accurate RP-HPLC method has been developed and validated for simultaneous estimation of Methylparaben (MP), Ketoconazole (KT), and Mometasone Furoate (MF) topical pharmaceutical dosage formulation. The separation was achieved by Waters X Terra C18 column using mobile phase consisting of buffer (triethyl amine in water, pH adjusted to 6.5 with glacial acetic acid)-acetonitrile (40 : 60, v/v) at a flow rate of 1.5 mL/min and detection at 250 nm. The method showed linearity with correlation coefficient <0.9999 over the range of 0.12–15.2 μg/mL, 0.67–149.4 μg/mL, and 0.42–7.6 μg/mL for MP, KT, and MF, respectively. The mean recoveries were found to be in the range of 99.9–101.1% for all the components. The method was validated as per the ICH guidelines for linearity, limit of detection, limit of quantification, accuracy, precision, robustness and solution stability. Stability indicating capability of the developed method was established by analyzing forced degradation of samples in which spectral purity of MP, KT, and MF along with separation of degradation products from analytes peak was achieved. The method can be successfully applied for routine analysis of quantitative determination of MP, KT, and MF in pharmaceutical dosage form.

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