scholarly journals Development and Validation of a Stability-Indicating HPLC Method for Empagliflozin and Linagliptin in Tablet Dosage Form

2021 ◽  
Vol 33 (2) ◽  
pp. 484-488
Author(s):  
Wael Abu Dayyih ◽  
Israa Al Ani ◽  
Ramadan I. Al-Shdefat ◽  
Zainab Zakareia ◽  
Sarah Ali Hamid ◽  
...  
Keyword(s):  
High Performance ◽  
Dosage Forms ◽  
Hplc Method ◽  
Forced Degradation ◽  
Solid Dosage Forms ◽  
Degradation Study ◽  
Stability Indicating ◽  
Solid Dosage ◽  
Development And Validation ◽  
Tablet Dosage

A simple, stability indicating high performance liquid chromatographical (HPLC) method was developed and validated for the estimation of empagliflozin and linagliptin in combined dosage forms. Chromatographical separation was optimized by isocratic HPLC using C-18 column [BDS 250 mm × 4.6 mm, 5 μm] utilizing a mobile phase consisting a mixuture of 0.1% orthophosphoric acid and acetonitrile (60:40 v/v) running at a rate of 1 mL/min and monitoring effluents at 230 nm. The retention time of empagliflozin and linagliptin was 2.05 min and 4.10 min, respectively. Correlation coefficient (r2) was 0.999 for both empagliflozin and linagliptin. The precision of method for the analysis of empagliflozin and linagliptin were 0.33 and 0.22, respectively. The accuracy of method (as recovery) was 100.96 to 101.48% for empagliflozin and 100.09 to101.13% for linagliptin. The results indicate the present method is accurate, precision and rugged as these results are within the specified limits. Therefore, the validated economical methodology can be applied for forced degradation study of empagliflozin and linagliptin in solid dosage forms.

scholarly journals Development and Validation of Stability Indicating RP-HPLC Method for the Estimation of Cinacalcet Hydrochloride in Bulk and Their Formulations

2020 ◽  
Vol 10 (6) ◽  
pp. 6610-6618
Keyword(s):  
Dosage Forms ◽  
Hplc Method ◽  
Forced Degradation ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Cinacalcet Hydrochloride ◽  
Development And Validation ◽  
Tablet Dosage

A Simple, selective, accurate, precise, linear, and stability-indicating RP-HPLC method was developed and validated for the estimation of Cinacalcet hydrochloride in bulk and tablet dosage forms. Chromatographic separation was achieved on X-Terra Symmetry C18 (4.6 x 150mm; 5 m) with mobile phase containing Phosphate buffer: Acetonitrile (40:60 v/v) pH adjusted to 3.0 ±0.05 with diluted ortho-phosphoric acid. The flow rate was maintained at 0.9 mL/min. The eluent was monitored at 282 nm. Moreover, the retention time of Cinacalcet was 2.8 minutes. The method was validated for linearity, accuracy, precision, and robustness as per ICH guidelines. The developed method was found linear between 25-150 μg/ml, and the linear regression coefficient was 0.999. The % RSD values are less than 2 % indicating the accuracy and precision of the method. The percentage of recovery was obtained from 98-102%. The system suitability parameters were found to be within the limit. Forced degradation studies were conducted under various conditions. The proposed method is simple, rapid, precise, and accurate. It can be used for the quantitation of Cinacalcet hydrochloride in bulk and commercial pharmaceutical dosage forms.

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 Development and validation of a novel stability indicating HPLC method for the separation and determination of darolutamide and its impurities in pharmaceutical formulations

2021 ◽  
Vol 104 (4) ◽  
pp. 57-68
Author(s):  
V.G. Kamani ◽  
◽  
M. Sujatha ◽  
G.B. Daddala ◽  
◽  
...  
Keyword(s):  
Ammonium Acetate ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Forced Degradation ◽  
Degradation Study ◽  
Stability Indicating ◽  
System Suitability ◽  
Development And Validation ◽  
First Time

This study reports for the first time about a stability indicating RP-HPLC method for analysis of darolutamide and its impurities 1, 2, and 3 in bulk and formulations. The separation was achieved on Phenomenex column with Luna C18 (250 mm × 4.6 mm, 5 μm) as stationary phase, and 50 mM ammonium acetate: methanol solution 15:80 (v/v) at pH 5.2 as mobile phase at 1.0 mL/min flow rate. UV detection was carried at wavelength of 239 nm. In these conditions the retention time of darolutamide and its impurities 1, 2, and 3 was 7.05, 8.90, 4.63 and 5.95 min, respectively. The method was validated for system suitability, range of analysis, precision, specificity, stability, and robustness. Forced degradation study was done through exposure of the analyte to five different stress conditions and the % degradation was small in all degradation condition. The proposed method can separate and estimate the drug and its impurities in pharmaceutical formulations. Hence, the developed method was suitable for the quantification of darolutamide and can separate and analyse impurities 1, 2, and 3

DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD FOR ESTIMATION OF EDOXABAN TOSYLATE IN TABLET DOSAGE FORMS

INDIAN DRUGS ◽  
2020 ◽  
Vol 57 (07) ◽  
pp. 47-51
Author(s):  
B. Anupama ◽  
P. Tejaswi ◽  
KNV. Chenchu Lakshmi ◽  
A. Vishwanadh
Keyword(s):  
High Performance ◽  
Reversed Phase ◽  
Dosage Forms ◽  
Hplc Method ◽  
Control Analysis ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Development And Validation ◽  
Tablet Dosage ◽  
Isocratic Mode

A rapid, simple and precise reversed phase high performance liquid chromatography (RP-HPLC) method was developed for the estimation of edoxabantosylate in tablets. The quantification was carried out using a Phenomenex C-18 column (250×4.6 mm i.d., 5µm particle size) in isocratic mode with mobile phase comprising of ammonium acetate buffer andacetonitrile in the ratio of 50:50 (V/V) at a flow rate 1 mL/min. The eluent was monitored at 240 nm. The retention time of the drug was 3.486 min. The calibration curve was linear in the concentration range of 5-25 µg/mL and per cent recovery ranged from 98.25-101.6.The developed method was validated as per ICH guidelines and the results obtained were satisfactory.The method can be applied for routine quality control analysis of edoxabantosylate in tablet dosage forms.

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 DEVELOPMENT AND VALIDATION OF STABILITY INDICATING CHROMATOGRAPHIC METHOD FOR SIMULTANEOUS ESTIMATION OF SACUBITRIL AND VALSARTAN IN PHARMACEUTICAL DOSAGE FORM

2017 ◽  
Vol 9 (5) ◽  
pp. 1
Author(s):  
Shweta Mishra ◽  
C. J. Patel ◽  
M. M. Patel
Keyword(s):  
Dosage Form ◽  
Degradation Products ◽  
Potassium Phosphate ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Development And Validation ◽  
Tablet Dosage

Objective: This study aims to develop and validate a stability indicating HPLC method for simultaneous estimation of sacubitril and valsartan in pharmaceutical dosage form.Methods: Sacubitril and valsartan separation were achieved by LC-20 AT C18 (250 mm x 4.6 mm) column and buffer (potassium phosphate, pH 3.0): methanol (50:50) as mobile phase, at a flow rate of 1 ml/min (millilitre per minute). Detection was carried out at 224 nm (nanometer). The different HPLC experimental parameters were optimized and the method was validated according to the standard guideline. Forced degradation experiments were carried out by exposing sacubitril and valsartan standard and sample for thermal, photolytic, oxidative and acid-base hydrolytic stress conditions.Results: Retention time of sacubitril and valsartan were found to be 4.170 min (minute) and 6.530 min (minute) respectively. The method has been validated for linearity, accuracy, precision, LOD, and LOQ. Linearity observed for sacubitril is 12.25-36.75 μg/ml (microgram per milliliter) and for valsartan is 12.75-38.25 μg/ml (microgram per milliliter). The results showed that sacubitril and valsartan and the other degradation products were fully resolved and thus the proposed method is stability-indicating.Conclusion: The proposed HPLC method was found to be simple, specific, precise, accurate, rapid and economical for simultaneous estimation of valsartan and sacubitril in bulk and tablet dosage form. Thus the validated economical method was applied for forced degradation study of sacubitril and valsartan tablet.

scholarly journals Development and Validation of a Stability-Indicating RP-HPLC Method for the Simultaneous Determination of Sofosbuvir, Velpatasvir, and Voxilaprevir in Tablet Formulation

2020 ◽  
pp. 7-14
Author(s):  
Deepthi R ◽  
Gowri Sankar D
Keyword(s):  
High Performance ◽  
Hplc Method ◽  
Solution Stability ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Development And Validation ◽  
Tablet Dosage ◽  
Optimized Conditions

Objective: The present study aimed to develop a stability-indicating reverse-phase high performance-liquid chromatography (RP-HPLC) method for the estimation of Sofosbuvir, Velpatasvir, and Voxilaprevir in tablet dosage form and validated in accordance with ICH guidelines. Methods: The optimized conditions for the developed RP-HPLC method are Agilent C18 (250 mm×4.6mm, 5μ) column maintained at 30ºC with a mobile phase consisting of Buffer(0.1%OPA) and Acetonitrile taken in the ratio 55:45%v/v on isocratic mode at flow rate 1.0ml/min. The sample was detected at 220 nm. Results: The retention time of Sofosbuvir, Velpatasvir, and Voxilaprevir was found to be 2.17, 2.731 and 3.55 min respectively. The developed method was validated for accuracy, precision, specificity, ruggedness, robustness and solution stability.

scholarly journals DEVELOPMENT AND VALIDATION OF A STABILITY INDICATING ASSAY FOR AZILSARTAN KAMEDOXOMIL IN SOLID DOSAGE FORMS.

2016 ◽  
Vol 4 (10) ◽  
pp. 1630-1639
Author(s):  
MohamedA. Kassem ◽  
◽  
MagdyI. Mohamed ◽  
AsmaaA. Mohamed ◽  
◽  
...  
Keyword(s):  
Dosage Forms ◽  
Solid Dosage Forms ◽  
Stability Indicating ◽  
Solid Dosage ◽  
Development And Validation

DEVELOPMENT AND VALIDATION OF RP-HPLC-PDA METHOD FOR THE ESTIMATION OF FENSPIRIDE HYDROCHLORIDE IN BULK AND PHARMACEUTICAL DOSAGE FORMS.

INDIAN DRUGS ◽  
2015 ◽  
Vol 52 (01) ◽  
pp. 20-25
Author(s):  
S. M Samyuktha ◽  
◽  
P. G Prasanthi ◽  
K Mahesh ◽  
B. N Nalluri ◽  
...  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Dosage Forms ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Development And Validation ◽  
Tablet Dosage ◽  
Liquid Chromatographic

A simple, selective, accurate High Performance Liquid Chromatographic (HPLC) method was developed and validated for the analysis of Fenspiride hydrochloride in bulk and tablet dosage forms. Chromatographic separation was achieved isocratically using a C18 reverse phase column [Inertsil C18 column (250×4.6mm, 5μm)] utilizing a mobile phase containing 10mM Ammonium acetate: Acetonitrile (50:50 v/v) at a flow rate of 1 mL/min. The eluents were monitored at wavelength of 210 nm for a run time of 7 minutes at ambient temperature. The average retention time of the drug was found to be 4.6 minutes. The developed method was validated as per ICH guidelines to ascertain the reproducibility of the method. The method was found to be linear in the concentration range of 10-50 μg/mL with a good correlation coefficient of 0.998. The limit of detection (LOD) and limit of quantification (LOQ) were 0.007 and 0.021 μg/mL and the percentage recovery and assay were found to be 99.315 and 98.97%. Specificity with placebo by 3 D plots showed that the method was specific and free from interfering substances. Therefore, the fully validated method was good enough to carry out routine analysis of Fenspiride in bulk and tablet formulations.

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