scholarly journals QUANTIFICATION OF ROPINIROLE HYDROCHLORIDE IN API AND TABLETS BY NOVEL STABILITY-INDICATING RP-HPLC METHOD: IT’S VALIDATION AND FORCED DEGRADATION STUDIES

2019 ◽  
pp. 293-298
Author(s):  
SADASHIVAIAH R. ◽  
Rohith G. ◽  
SATHEESHA BABU B. K.
Keyword(s):  
Retention Time ◽  
High Performance ◽  
Human Error ◽  
Hplc Method ◽  
Forced Degradation ◽  
Chromatography Method ◽  
Stability Indicating ◽  
Forced Degradation Studies ◽  
Ropinirole Hydrochloride ◽  
Degradation Studies

Objective: A simple, economical, robust and stability-indicating reverse phase high performance liquid chromatography method was developed and validated for the quantification of ropinirole hydrochloride in API and tablets to achieve shorter retention time, to minimize human error by avoiding the use of buffers and weighing procedure and analyze more number of samples in shorter period of time with good accuracy. Methods: The chromatographic conditions for separation of ropinirole hydrochloride was carried out using Gemini NX C18 column (15 cm x 4.6 mm), 5 µm particle size with the mobile phase composing of methanol: acetonitrile (70:30 v/v), delivered at flow rate 0.7 ml/min and UV detection wavelength at 250 nm. Results: The retention time was observed at 2.718 min. The system suitability results were found to be within limits. The method was precise, with lower than 2 %RSD and the calibration curve was linear (r2=1) over a concentration range of 2.5-160 µg/ml. The detection and quantification limit was found to be 0.045 µg/ml and 0.15 µg/ml, respectively. Recovery of the drug was found between 100.09-100.19%. The assay of ropinirole hydrochloride in ROPITOR® and ROPARK® tablets were found to be 100.4 and 103.60 %, respectively. The forced degradation studies were carried out to demonstrate the specificity of the method by exposing the API under conditions of hydrolysis, oxidation, thermal and photolytic as per ICH Q1A(R2) guidelines. Conclusion: The low coefficient of variation and agreeable recovery confirmed that the newly developed method could be employed for routine analysis of ropinirole hydrochloride in API and tablets.

scholarly journals Stability indicating thin-layer chromatographic method for estimation of antidiabetic drug Remogliflozin etabonate

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Dimal A. Shah ◽  
Ishita I. Gondalia ◽  
Vandana B. Patel ◽  
Ashok Mahajan ◽  
Usmangani Chhalotiya ◽  
...  
Keyword(s):  
Thin Layer ◽  
High Performance ◽  
Chromatographic Method ◽  
Tablet Formulation ◽  
Base Hydrolysis ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Forced Degradation Studies ◽  
Degradation Studies ◽  
Remogliflozin Etabonate

Abstract Background A sensitive, precise, and stability-indicating high-performance thin-layer chromatographic (HPTLC) method has been developed for the analysis of Remogliflozin etabonate in tablet formulation. HPTLC plates precoated with silica gel 60 F254 were used as the stationary phase; methanol: ethyl acetate: toluene: NH3 (2:4:4:0.1, v/v/v) was used as mobile phase, and densitometry was used for the quantitative estimation of the drug. The proposed method was validated with respect to linearity, accuracy, precision, and robustness and applied for the estimation of drug in tablet dosage form. Results The Rf value of Remogliflozin etabonate was observed to be 0.61. The densitometric estimation was performed in reflectance mode at 229 nm. The method was found to be linear in the range of 500–8000 ng/band for Remogliflozin etabonate. The possible degradation pathway was estimated by performing forced degradation studies. The degradant peaks were well resolved from the drug peak with acceptable resolution in their Rf value. Conclusion An accurate and precise high-performance thin-layer chromatographic method has been developed for the quantification of Remogliflozin etabonate in tablets. Forced degradation studies were performed, and drug was found to be highly susceptible to acid, base hydrolysis, and oxidative stress degradation and gets converted into active drug Remogliflozin. Both Remogliflozin etabonate and Remogliflozin bands were well resolved. The method was applied for the analysis of drug in tablet formulation, and it can be used for routine quality control analysis, as well as for the analysis of stability samples.

scholarly journals STABILITY INDICATING RP-HPLC ASSAY METHOD FOR ESTIMATION OF DIMETHYL FUMARATE IN BULK AND CAPSULES

2017 ◽  
Vol 9 (5) ◽  
pp. 121 ◽  
Author(s):  
Hemant K. Jain ◽  
Archana A. Gunjal
Keyword(s):  
Dimethyl Fumarate ◽  
Hplc Method ◽  
Assay Method ◽  
Forced Degradation ◽  
Dihydrogen Phosphate ◽  
Column Temperature ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Forced Degradation Studies ◽  
Degradation Studies

Objective: To develop an accurate, simple, precise and specific stability indicating RP-HPLC method for estimation of dimethyl fumarate in bulk and capsules.Methods: An Inertsil ODS (150x4.6 mm, 5µ) column and a mobile phase containing acetonitrile: potassium dihydrogen phosphate buffer pH 6.8 (50:50% v/v) was used for this study. The flow rate was maintained at 1.0 ml/min; column temperature was fixed at 35 °C and UV detection was carried out at 210 nm. The forced degradation studies were performed and method was validated with as per ICH guidelines.Results: The retention time of dimethyl fumarate was found to be 3.3±0.02 min. The value of correlation coefficient between peak area and concentration was found to be 0.9993. The mean percent recovery of dimethyl fumarate in capsules was found in the range of 99.65 to 101.64%. The results of forced degradation studies indicated that the drug was found to be stable in basic, oxidative and thermal conditions while degraded in acidic conditions.Conclusion: It can be conducted from results that the developed HPLC method is simple, accurate, precise and specific. Results of stress testing study revealed that the method is stability indicating. Thus, this method can be used for routine analysis of dimethyl fumarate capsules and check their stability.  

scholarly journals Development and Validation of Stability-Indicating Reverse Phase-High Performance Liquid Chromatography Method for Simultaneous Determination of Atenolol and Nifedipine in Bulk and Tablet Dosage Form

2020 ◽  
Vol 11 (02) ◽  
pp. 219-223
Author(s):  
Ansari Yaasir Ahmed ◽  
Qazi Shoeb ◽  
Umme Rumana ◽  
Patel Afroza ◽  
Pathan Vahid Tajkhan ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Forced Degradation ◽  
Chromatography Method ◽  
Stability Indicating ◽  
Limit Of Quantitation

The new stability-indicating high performance liquid chromatography (HPLC) method has been developed and validated with different parameters for atenolol (ATE) and nifedipine (NIFE) in the combined dosage form. The chromatographic conditions were optimized using a mobile phase of MeOH:OPA (70:30) with a flow rate of 0.7 mL/min. Column (C18) of 4.6 × 250 mm dimension was used as a stationary phase; the particle size capacity of the column was 5 μm. The detection was carried out at 233 nm. The method was validated according to ICH guidelines for linearity, precision, repeatability, the limit of detection (LoD), and limit of quantitation (LoQ). The response was found to be linear in the concentration range of 20 to 100 mcg/mL for ATE and 1 to 5 mcg/mL for NIFE. The developed method shows the minimum quantity of drugs to be identified (LoD) and minimum drug to be quantified (LoQ). The LoD and LoQ were found to be 0.1415 and 0.4289, respectively, for ATE, and 0.1834 and 0.5558, respectively, for NIFE. The method was linear, simple, precise, and accurate and, therefore, suitable for routine analysis of drugs in tablet form. The forced degradation studies were also done through the exposure of analyte solution to four different stress conditions.

scholarly journals DEVELOPMENT OF FORCED DEGRADATION STUDIES OF FAVIPIRAVIR BY RP-HPLC

2021 ◽  
Vol 10 (6) ◽  
pp. 3823-3826
Author(s):  
, Shyamala
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Ultra Violet ◽  
Active Pharmaceutical Ingredient ◽  
Spectral Studies ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Forced Degradation Studies ◽  
Degradation Studies

Forced degradation studies and stability indicating method were developed for the estimation of Favipiravir by reverse phase High performance liquid chromatography in active Pharmaceutical ingredient and its tablet dosage form. The method was achieved by using C18 column (250 X 4.6mm X 4µm) with mobile phase mixture ortho phosphoric acid and acetonitrile in the ratio 60:40. The mobile phase was allowed to pump with the flow rate 1ml/min by maintaining detection wavelength at 324nm using ultra-violet detector. Favipiravir drug was subjected to various stress conditions according to International Conference of Harmonization Q1A(R2) guidelines to establish stability indicating method. Favipiravir drug was found to be sensitive at peroxide degradation. The impurity peak was characterized by mass spectral studies. The method was validated for analytical standards such as linearity, accuracy, Precision, sensitivity and robustness. A rapid and sensitive method was developed for the estimation of favipiravir which indicates its stability indicating behavior.

DEVELOPMENT AND VALIDATION OF A STABILITY-INDICATING RP-HPLC METHOD FOR ESTIMATION OF AMBRISENTAN AND ITS PROCESS-RELATED IMPURITIES IN BULK AND PHARMACEUTICAL DOSAGE FORMS

INDIAN DRUGS ◽  
2015 ◽  
Vol 52 (12) ◽  
pp. 34-41
Author(s):  
S. K Kondila ◽  
◽  
K Sujana ◽  
A Prameela Rani
Keyword(s):  
High Performance ◽  
Reversed Phase ◽  
Dosage Forms ◽  
Hplc Method ◽  
Forced Degradation ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Photolytic Degradation ◽  
Acid And Base

The aim of the present work was to develop and validate an accurate, precise, simple, and efficient stability indicating Reversed phase High Performance Liquid Chromatography method for determination of an abrisentan and its process impurities in bulk and pharmaceutical dosage forms. The drug substance was subjected to stress conditions such as hydrolysis (acid and base), oxidation, photolysis and thermal degradation as per International Conference on Harmonization guidelines to study the stability-indicating profile of drug. Significant degradation was observed during acid hydrolysis and peroxide degradation. The chromatographic conditions were optimized using an impurity-spiked solution and samples generated from forced degradation studies. The method was developed using Agilent XDB-C18 (150×4.5mm, 5μ) column and 10mM NH4OAc (pH-5.2 adjusted with acetic acid): ACN as the mobile phase with gradient programme at a flow rate of 1 mL/min. effluents were monitored at 289 nm. The retention times were found as 25.945 min for IMP-1, 24.685 min for IMP-2, 23.83 min for IMP-3, 10.53 min for AMB, 5011 min for IMP-4 and 3.48 min for IMP-5. The mean recovery values were found to be 98.52-100.44% for AMD and its impurities. The degradation rate of AMB in acid, base, peroxide (oxidative) thermal and photolytic degradation processes was found in range 7-22%. The developed analytical method has been validated for specificity, linearity, precision, accuracy, and robustness which were within the acceptance limit according to ICH guidelines. The developed method was successfully employed for routine quality control and stability analysis of AMB in pharmaceutical dosage forms.

scholarly journals Forced degradation of tacrolimus and the development of a UHPLC method for impurities determination

2019 ◽  
Vol 69 (3) ◽  
pp. 363-380 ◽  
Author(s):  
Tanja Rozman Peterka ◽  
Tina Trdan Lušin ◽  
Jure Bergles ◽  
Zoran Ham ◽  
Rok Grahek ◽  
...  
Keyword(s):  
High Performance ◽  
Gradient Elution ◽  
Dosage Forms ◽  
Forced Degradation ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Forms ◽  
Thermal Light ◽  
Forced Degradation Studies ◽  
Degradation Studies ◽  
Liquid Chromatography Method

Abstract An ultra-high performance liquid chromatography method for simultaneous determination of tacrolimus impurities in pharmaceutical dosage forms has been developed. Appropriate chromatographic separation was achieved on a BEH C18 column using gradient elution with a total run time of 14 min. The method was applied to analyses of commercial samples and was validated in terms of linearity, precision, accuracy, sensitivity and specificity. It was found to be linear, precise and accurate in the range of 0.05 to 0.6 % of the impurities level in pharmaceutical dosage forms. Stability indicating power of the method was demonstrated by the results of forced degradation studies. The forced degradation study in solution revealed tacrolimus instability under stress alkaline, thermal, light and photolytic conditions and in the presence of a radical initiator or metal ions. The drug was stable at pH 3–5. Solid-state degradation studies conducted on amorphous tacrolimus demonstrated its sensitivity to light, elevated temperature, humidity and oxidation.

scholarly journals Development and Validation of RP-HPLC Assay Method for Vildagliptin Using Qbd Approach and Its Application to Forced Degradation Studies

2016 ◽  
Vol 8 (03) ◽  
Author(s):  
Meetali M. Chaphekar ◽  
Purnima Hamrapurkar
Keyword(s):  
Method Development ◽  
Accurate Determination ◽  
Interaction Effects ◽  
Hplc Method ◽  
Assay Method ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Forced Degradation Studies ◽  
Degradation Studies

The concept of Quality by design (QbD) has recently gained importance in the area of analytical method development and involves understanding of the critical factors and their interaction effects by a desired set of experiments. So, the present work describes the development of Reverse Phase-High Performance Liquid Chromatography (RP-HPLC) method by QbD approach using Design of Experiments and subsequent validation for analysis of Vildagliptin in bulk drug and its pharmaceutical formulation. An efficient experimental design based on systematic scouting of all three key components of the RP‐HPLC method (Buffer pH, Organic Phase-% acetonitrile, Organic Modifier-Methanol) is presented. The significance and interaction effects of these parameters on the response variables (Retention time and tailing factor) were evaluated through statistical analysis tools like Analysis of Variance (ANOVA) and plots which revealed the final chromatographic conditions of the method. The developed method was validated and Forced degradation studies were also carried out in order to determine the stability-indicating nature of the method. The chromatographic separation was achieved on Jasco CrestPack RP C18 (250 × 4.6 mm, 5μ) column using Buffer (pH 6): Acetonitrile: Methanol (70:10:20 v/v) as mobile phase and detection was done using Photo-Diode Array (PDA) detector at 210 nm. The developed method of Vildagliptin is linear over a range of 5-15μg/ml having correlation coefficient R2 value as 0.999. The %RSD for precision and accuracy of the method was found to be less than 2%. Forced Degradation studies revealed that the method was found to be stability-indicating. The results showed that the proposed method is suitable for the precise and accurate determination of Vildagliptin in bulk and its formulation.

scholarly journals RP-HPLC METHOD DEVELOPMENT AND VALIDATION FOR SIMULTANIOUS ESTIMATION AND FORCED DEGRADATION STUDIES OF LAMIVUDINE AND RALTEGRAVIR IN SOLID DOSAGE FORM

2018 ◽  
Vol 10 (6) ◽  
pp. 242
Author(s):  
Juluri Krishna Dutta Tejaswi ◽  
R. Govinda Rajan
Keyword(s):  
Correlation Coefficient ◽  
High Performance ◽  
Dosage Form ◽  
Method Development ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Rp Hplc ◽  
Forced Degradation Studies ◽  
Degradation Studies

Objective: A stability indicating reverse phase high-performance liquid chromatography (RP-HPLC) method was developed and validated for the estimation of the combined tablet formulation of lamivudine (LAM) and raltegravir (RAL) in dosage forms and its API.Methods: Chromatographic separation was achieved on inertsil ODS C18 5 µm (4.6 X 150 mm) using a mobile phase (MP) consisting of a mixture of mixed orthophosphoric acid (OPA): acetonitrile (ACN) in the ratio 50:50 v/v which was determined at 242 nm respectively. Results: The assay of LAM and RAL was performed with tablets, and the % assay was found to be 100.12 and 99.89 which shows that the method is useful for routine analysis. The linearity of LAM and RAL was found to be linear with a correlation coefficient of 0.998 and 0.999, which shows that the method is capable of producing good sensitivity. The retention time of LAM and RAL was 1.99 min and 4.34 min respectively; linearity range was found to lie from 15 µg/ml to 75 µg/ml for LAM, 30 µg/ml to 150 µg/ml for RAL with a correlation coefficient of 0.999 respectively. Forced degradation studies were conducted in acidic, basic, thermal, photolytic and peroxide where all the degradation peaks were monitored.Conclusion: The proposed HPLC method was found to be simple, specific, precise, accurate, rapid and economical for simultaneous estimation of LAM and RAL in bulk and tablet dosage form. Thus the validated economical method was applied for forced degradation study of LAM and RAL tablet.

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