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

scholarly journals Development and Validation of Stability Indicating RP-HPLC Method for the Determination of Metaxalone in Bulk and its Pharmaceutical Formulations

2011 ◽  
Vol 8 (s1) ◽  
pp. S439-S447 ◽  
Author(s):  
Prafulla Kumar Sahu ◽  
M. Mathrusri Annapurna ◽  
Sahoo Dillip Kumar
Keyword(s):  
Dynamic Range ◽  
Internal Standard ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Standard Curve ◽  
Oxidation Reduction ◽  
Development And Validation

A stability indicating reverse phase HPLC method was developed for the determination of metaxalone, a skeletal muscle relaxant, present in bulk and its pharmaceutical formulations using gliclazide as the internal standard (I.S). A hypersil ODS C18 column (250 × 4.6 mm, packed with 5 micron) in an isocratic mode with mobile phase Acetonitrile: phosphate buffer 3.6 (50:50%v/v) was used at a flow rate of 0.8 mL/ min and effluent was monitored at 225 nm. The assay exhibited a linear dynamic range of 0.6-100 µg/mL. Acceptable precision and accuracy were obtained for concentrations over the standard curve range. The retention times were 5.13 min and 9.08 min for metaxalone and IS respectively. The extraction recovery of metaxalone from pharmaceutical dosage form (tablets) was >97% and the calibration curve was linear (r2= 0.999) over the entire linear range. The method had an accuracy of >98% and LOD and LOQ of 0.2 µg/mL and 0.6 µg/mL respectively. The specificity of the proposed method was performed whereby metaxalone undergoes different stress conditions like oxidation, reduction, photolysis, acid and alkaline hydrolysis.

scholarly journals Development and validation of a stability indicating RP-HPLC-DAD method for the determination of bromazepam

PLoS ONE ◽  
2021 ◽  
Vol 16 (3) ◽  
pp. e0244951
Author(s):  
Hany W. Darwish ◽  
Nesma A. Ali ◽  
Ibrahim A. Naguib ◽  
Mohamed R. El Ghobashy ◽  
Abdullah M. Al-Hossaini ◽  
...  
Keyword(s):  
Hplc Method ◽  
Array Detector ◽  
Forced Degradation ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Photodiode Array Detector ◽  
Alkaline Conditions ◽  
Development And Validation

A reliable, selective and sensitive stability-indicating RP-HPLC assay was established for the quantitation of bromazepam (BMZ) and one of the degradant and stated potential impurities; 2-(2-amino-5-bromobenzoyl) pyridine (ABP). The assay was accomplished on a C18 column (250 mm × 4.6 mm i.d., 5 μm particle size), and utilizing methanol-water (70: 30, v/v) as the mobile phase, at a flow rate of 1.0 ml min-1. HPLC detection of elute was obtained by a photodiode array detector (DAD) which was set at 230 nm. ICH guidelines were adhered for validation of proposed method regarding specificity, sensitivity, precision, linearity, accuracy, system suitability and robustness. Calibration curves of BMZ and ABP were created in the range of 1–16 μg mL-1 with mean recovery percentage of 100.02 ± 1.245 and 99.74 ± 1.124, and detection limit of 0.20 μg mL-1 and 0.24 μg mL-1 respectively. BMZ stability was inspected under various ICH forced degradation conditions and it was found to be easily degraded in acidic and alkaline conditions. The results revealed the suitability of the described methodology for the quantitation of the impurity (ABP) in a BMZ pure sample. The determination of BMZ in pharmaceutical dosage forms was conducted with the described method and showed mean percentage recovery of 99.39 ± 1.401 and 98.72 ± 1.795 (n = 6), respectively. When comparing the described procedure to a reference HPLC method statistically, no significant differences between the two methods in regard to both accuracy and precision were found.

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 the stability-indicating LC-UV method for the determination of cefoselis sulphate

2012 ◽  
Vol 10 (1) ◽  
pp. 121-126 ◽  
Author(s):  
Przemysław Zalewski ◽  
Judyta Cielecka-Piontek ◽  
Anna Jelińska
Keyword(s):  
Mobile Phase ◽  
Degradation Products ◽  
Kinetic Studies ◽  
Hplc Method ◽  
Assay Method ◽  
Forced Degradation ◽  
Stability Indicating ◽  
The Stability ◽  
Development And Validation

AbstractThe stability-indicating LC assay method was developed and validated for quantitative determination of cefoselis sulphate in the presence of degradation products formed during the forced degradation studies. An isocratic, RP-HPLC method was developed with C-18 (250 × 4.6 mm, 5 µm) column and 12 mM ammonium acetate-acetonitrile (95:5 V/V) as a mobile phase. The flow rate of the mobile phase was 1.0 mL min−1. Detection wavelength was 260 nm and temperature was 30°C. Cefoselis similarly to other cephalosporins was subjected to stress conditions of degradation in aqueous solutions including hydrolysis, oxidation, photolysis and thermal degradation. The developed method was validated with regard to linearity, accuracy, precision, selectivity and robustness. The method was applied successfully for identification and determination of cefoselis sulphate in pharmaceuticals and during kinetic studies.

Development and Validation of Stability Indicating RP-HPLC Method for Determination of Enzalutamide

2019 ◽  
Vol 12 (5) ◽  
pp. 4635-4645
Author(s):  
Pankaj Padmakar Nerkar ◽  
Sameer Ansari ◽  
Shailesh Chalikwar
Keyword(s):  
Ammonium Acetate ◽  
Correlation Coefficients ◽  
Reversed Phase ◽  
Hplc Method ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Development And Validation

A simple, isocratic, and accurate reversed phase HPLC method was developed for the quantitative determination of enzalutamide. The chromatographic separation was achieved on an Qualisil BDS C18 (250 mm x 4.6mm, 5 μm) column using methanol: ammonium acetate buffer pH 4.2 adjusted with glacial acetic acid: (60:40, v/v) as a mobile phase, at a flow rate of 1 ml/min and detection at 236nm. The linear range for enzalutamide were 2.0 to        10 μg/mL was obtained with correlation coefficients ≥ 0.998. The retention time was found to be 6.30min. Enzalutamide was subjected to stress conditions hydrolysis (acid, base) oxidation, photolysis and thermal degradation and the stressed samples were analysed by the developed method. The method was validated for the precision, accuracy, linearity and robustness. The developed stability indicating method for enzalutamide was validated as per ICH guidelines.

A New Validated Stability Indicating RP-HPLC Method for the Quantification of Allopurinol and Lesinurad in Bulk and Pharmaceutical Formulations

2020 ◽  
Vol 5 (1) ◽  
pp. 51-55
Author(s):  
K.V. Ramanjaneyulu ◽  
K. Venkata Ramana ◽  
M. Prasada Rao
Keyword(s):  
Degradation Products ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Forced Degradation ◽  
Analysis Method ◽  
Degradation Study ◽  
Stability Indicating ◽  
Stress Study ◽  
Isocratic Hplc ◽  
Bulk Drug

The objective of this study was to develop and validate a method for simultaneous quantitative analysis of allopurinol and lesinurad in bulk drug and pharmaceutical formulations. An isocratic HPLC analysis method using a reverse phase Waters spherisorb ODS1 C18 column (250 mm × 4.6 mm, 5 μ) and a simple mobile phase without buffer was developed, optimized and fully validated. Analyses were carried out at a flow rate of 0.9 mL/min at 50 °C and monitored at 246 nm. This HPLC method exhibited good linearity, accuracy and selectivity. The recovery (accuracy) of both allopurinol and lesinurad from all matrices was greater than 98 %. The allopurinol and lesinurad peak detected in the samples of a forced degradation study and no interference of excepients or the degradation products formed during stress study. The method was rugged with good intra- and inter-day precision and sensitive. This stability indicating HPLC method was selective, accurate and precise for the simultaneous analysis of allopurinol and lesinurad in pharmaceutical formulations.

A Stability-Indicating HPLC Method for the Quantification of Aliskiren and Hydrochlorothiazide in a Pharmaceutical Formulation

2014 ◽  
Vol 97 (6) ◽  
pp. 1519-1525 ◽  
Author(s):  
Dimitrios Karvelis ◽  
Eleni Kalogria ◽  
Irene Panderi
Keyword(s):  
Ammonium Acetate ◽  
Degradation Products ◽  
Hplc Method ◽  
Percentage Error ◽  
Forced Degradation ◽  
Content Uniformity ◽  
Isocratic Elution ◽  
Stability Indicating ◽  
Relative Percentage Error

Abstract A novel, fast, and sensitive stability-indicating HPLC method was developed, fully validated, and applied to the simultaneous determination of aliskiren and hydrochlorothiazide in a combined formulation. Effective chromatographic separation was achieved using a phenyl analytical column with isocratic elution using the mobile phase 0.030 M ammonium acetate–acetonitrile (60 + 40, v/v) at a flow rate of 0.40 mL/min. The UV spectrophotometric detector was set at 280 nm. The method was linear over the concentration ranges of 1.5–4.5 and 0.125–0.375 μg/mL for aliskiren and hydrochlorothiazide, respectively. The intraday and interday RSD values were less than 6.1%, while the relative percentage error, Er, was less than 5% for both analytes. Both drugs were subjected to stress conditions of acidic and alkaline hydrolysis, oxidation, and thermal degradation. The proposed method proved to be stability indicating by resolution of the drugs from their forced degradation products. The method was applied successfully to the QC and content uniformity tests in combined commercial tablets.

scholarly journals Development and validation of a new analytical RP-HPLC method for simultaneous determination of Glibenclamide and Atenolol in bulk

2019 ◽  
Vol 10 (3) ◽  
pp. 2433-2445
Author(s):  
Anitha P ◽  
Ramkanth S ◽  
Satyanarayana S V
Keyword(s):  
Hplc Method ◽  
Fixed Dose ◽  
Simultaneous Estimation ◽  
Uv Detector ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
System Suitability ◽  
Development And Validation ◽  
First Time

A new, simple, reliable, fast, sensitive and economical RP-HPLC method was developed and validated for simultaneous estimation of two fixed-dose combinations frequently prescribed in coexisted chronic diseases such as diabetes (GLB) and hypertension (ATN) in bulk for the first time. The mobile phase used for the chromatographic runs consisted of 0.01N potassium dihydrogen ortho phosphate (pH 4.8) and acetonitrile (55:45, v/v). The separation was achieved on column (BDS C18 250 x 2.1mm, 1.6m) using isocratic mode. Drug peaks were well separated and were detected by a UV detector at 235.0 nm. The method was linear at the concentration range 2.5-15µg/ml for Glibenclamide (GLB) and 6.25-37.5µg/ml for Atenolol (ATN), respectively. The method has been validated according to ICH guidelines with respect to system suitability, specificity, precision, accuracy and robustness. The method was validated for system suitability, linearity, accuracy, precision, detection, quantification limits and robustness and was found it is acceptable in the range of 2.5–15 µg/ml for GLB and 6.25–37.5 µg/ml for ATN. The LOD and LOQ of GLB was found to be 0.48 µg/ml and 1.47µg/ml and for ATN was found to be 0.72µg/ml and 2.20 µg/ml, respectively. The method was applied to drug interaction studies of GLB with ATN to illustrate the scope and application of the methods to manage two different therapeutic classes of drugs, as they may co-administered in concurrent diseases.

scholarly journals Development and Validation of a Stability Indicating RP-HPLC Method for the Determination of Two Sun Protection Factors (Koptrizon and Tinosorb S) in Topical Pharmaceutical Formulations Using Experimental Designs

2013 ◽  
Vol 2013 ◽  
pp. 1-12 ◽  
Author(s):  
Chinmoy Roy ◽  
Jitamanyu Chakrabarty
Keyword(s):  
Factorial Design ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Full Factorial Design ◽  
Plate Count ◽  
Forced Degradation ◽  
Solution Stability ◽  
Stability Indicating ◽  
Full Factorial

A novel, simple, validated stability indicating HPLC method was developed for determination of Koptrizon and Tinosorb S. Stability indicating power of the method was established by forced degradation study. The chromatographic separation was achieved with Waters X Bridge column, by using mobile phase consisting of a mixture of acetonitrile : tetrahydrofuran : water (38 : 38 : 24, v/v/v). The method fulfilled validation criteria and was shown to be sensitive, with limits of detection (LOD) and quantitation (LOQ) of 0.024 and 0.08 μg  for Koptrizon and 0.048 and 0.16 μg  for Tinosorb S, respectively. The developed method is validated for parameters like precision, accuracy, linearity, solution stability, specificity, and ruggedness as per ICH norms. Design expert with ANOVA software with linear model was applied and a 23 full factorial design was employed to estimate the model coefficients and also to check the robustness of the method. Results of the two-level full factorial design, 23 with 10 runs including two-centre-point analysis based on the variance analysis (ANOVA), demonstrated that all three factors, as well as the interactions between retention time of Koptrizon, Tinosorb S, and USP plate count for Koptrizon, are statistically significant.

Sign in / Sign up

Export Citation Format

Share Document