scholarly journals A Stability-Indicating HPLC-DAD Method for Determination of Stiripentol: Development, Validation, Kinetics, Structure Elucidation and Application to Commercial Dosage Form

2014 ◽  
Vol 2014 ◽  
pp. 1-10 ◽  
Author(s):  
Hany W. Darwish ◽  
Ali S. Abdelhameed ◽  
Mohamed I. Attia ◽  
Ahmed H. Bakheit ◽  
Nasr Y. Khalil ◽  
...  
Keyword(s):  
Degradation Product ◽  
Dosage Form ◽  
Reversed Phase ◽  
Stress Conditions ◽  
Array Detector ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Relative Standard

A rapid, simple, sensitive, and accurate isocratic reversed-phase stability-indicating high performance liquid chromatography method has been developed and validated for the determination of stiripentol and its degradation product in its bulk form and pharmaceutical dosage form. Chromatographic separation was achieved on a Symmetry C18 column and quantification was achieved using photodiode array detector (DAD). The method was validated in accordance with the ICH requirements showing specificity, linearity (r2=0.9996, range of 1–25 μg/mL), precision (relative standard deviation lower than 2%), accuracy (mean recovery100.08±1.73), limits of detection and quantitation (LOD = 0.024 and LOQ = 0.081 μg/mL), and robustness. Stiripentol was subjected to various stress conditions and it has shown marked stability under alkaline hydrolytic stress conditions, thermal, oxidative, and photolytic conditions. Stiripentol degraded only under acidic conditions, forming a single degradation product which was well resolved from the pure drug with significantly different retention time values. This degradation product was characterized by1H-NMR and13C-NMR spectroscopy as well as ion trap mass spectrometry. The results demonstrated that the method would have a great value when applied in quality control and stability studies for stiripentol.

scholarly journals Stability-indicating HPLC determination of ciprofibrate in bulk drug and pharmaceutical dosage form

2012 ◽  
Vol 18 (1) ◽  
pp. 95-101 ◽  
Author(s):  
P.S. Jain ◽  
H.N. Jivani ◽  
R.N. Khatal ◽  
S.J. Surana
Keyword(s):  
Dosage Form ◽  
Degradation Products ◽  
Reversed Phase ◽  
Stress Conditions ◽  
Assay Method ◽  
Main Peak ◽  
Forced Degradation ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating

A novel stability-indicating high-performance liquid chromatographic assay method was developed and validated for quantitative determination of ciprofibrate in bulk drugs and in pharmaceutical dosage form in the presence of degradation products. An isocratic, reversed phase HPLC method was developed to separate the drug from the degradation products, using an Ace5-C18 (250?4.6 mm, 5 ?m) advance chromatography column, and methanol and water (90:10 v/v) as a mobile phase. The detection was carried out at a wavelength of 232 nm. The ciprofibrate was subjected to stress conditions of hydrolysis (acid, base), oxidation, photolysis and thermal degradation. Degradation was observed for ciprofibrate in base, in acid and in 30% H2O2. The drug was found to be stable in the other stress conditions attempted. The degradation products were well resolved from the main peak. The percentage recovery of ciprofibrate was from (98.65 to 100.01%) in the pharmaceutical dosage form. The developed method was validated with respect to linearity, accuracy (recovery), precision, system suitability, specificity and robustness. The forced degradation studies prove the stability indicating power of the method.

scholarly journals Stability Indicating RP-HPLC Method For Determination Of Ketoconazole In Bulk Drug And In Tablet Dosage Form

2021 ◽  
Vol 001 (02) ◽  
Author(s):  
Shalin Parikh ◽  
Jayant Dave ◽  
Jayendrakumar Patel
Keyword(s):  
Dosage Form ◽  
Linear Regression Analysis ◽  
Hplc Method ◽  
Stress Conditions ◽  
Dihydrogen Phosphate ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Bulk Drug

A simple, precise, accurate and sensitive isocratic stability indicating RP-HPLC method has been developed and validated for determination of Ketoconazole in bulk drug and pharmaceutical dosage form. Isocratic RP-HPLC separation was achieved on Agilent C8 (150 mm ?4.6 mm, 5 µm particle size) with the mobile phase 0.3 % Triaethylamine in 20 mM potassium dihydrogen phosphate buffer pH adjusted to 4.0: Acetonitrile (68:32 % v/v) at a flow rate 1.0 ml/min. The retention time of Ketoconazole was 8.97 ± 0.50 min. The method was validated for specificity, linearity, precision, accuracy and robustness. The linear regression analysis data of calibration curve showed good linearity in concentration range 10-60 ?g/ml. The Intraday and Interday precision were 0.59-1.11 % and 0.26-1.73 % RSD respectively. The accuracy was found to be 98.11-99.26 %. The drug was subjected to the stress conditions like hydrolysis, oxidation, photolysis and dry heat. The proposed method is found to be specific with respect to degradation product formed after Acidic hydrolysis, Oxidation, Thermal and Photolytic degradation. The Ketoconazole was found to be stable under neutral hydrolytic, thermal and photolytic stress conditions. Acidic, thermal, photolytic stress conditions showed degradation. The proposed chromatographic method can be used for estimation of drug during stress testing & formal stability studies.

scholarly journals Stability Indicating HPLC Method for the Determination of Delamanid in Pharmaceutical Dosage Form

2021 ◽  
Vol 11 (1-s) ◽  
pp. 108-112
Author(s):  
Advaita B. Patel ◽  
Deepa R. Patel ◽  
Dhaval M. Patel ◽  
Mansi Babaria
Keyword(s):  
Analytical Method ◽  
Mobile Phase ◽  
Dosage Form ◽  
Degradation Products ◽  
Stress Test ◽  
Reversed Phase ◽  
Hplc Method ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating

Delamanid is successfully used for treatment of MDR TB. A stability indicating analytical method has been developed and validated. In this study Delamanid was degraded under different stress test conditions as per International Conference on Harmonization. The degraded samples were used to develop a stability-indicating high performance liquid chromatographic (HPLC) method for the Delamanid. The Delamanid was well separated from degradation products using a reversed-phase Hypersil BDS C18 (250 mm × 4.6mm i.d., 5µm) column and a mobile phase comprising of 0.01M pH 2.70 Phosphate Buffer: Acetonitrile (pH 3.50) 70:30, pH of mobile phase was adjusted with Glacial acetic acid and other HPLC parameters were flow rate 1 mL/min, detection wavelength 254 nm and injection volume 10 µl. The method was validated for linearity, precision, accuracy, ruggedness and robustness. Results obtained after validation study indicating that the proposed single method allowed analysis of Delamanid in the presence of their degradation products formed under a variety of stress conditions. The developed procedure was also applicable to the determination of stability of the Delamanid in commercial pharmaceutical dosage form. Keywords:  Delamanid, stability indicating analytical method, HPLC

DEVELOPMENT AND VALIDATION OF NOVEL STABILITY INDICATING RP-HPLC METHOD FOR QUANTIFICATION OF TOLVAPTAN IN BULK AND PHARMACEUTICAL DOSAGE FORM

INDIAN DRUGS ◽  
2020 ◽  
Vol 57 (03) ◽  
pp. 62-68
Author(s):  
Khaleel Noorbasha ◽  
S. K. Abdul Rahaman
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
Reversed Phase ◽  
Hplc Method ◽  
Working Standard ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Relative Standard ◽  
Bulk Drug

Specific stability-indicating reversed-phase high performance liquid chromatography (HPLC) method has been developed and validated for the quantification of tolvaptan in bulk drug and pharmaceutical dosage form. The optimized conditions for the developed HPLC method are; Inertil ODS-3V column (150 x 4.6 mm, 5.0 mm) maintained at 30°C with mobile phase consisting of 0.1% ortho phosphoric acid and acetonitrile in the ratio 40:60%v/v on isocratic mode at flow rate of 1.0 mL/min and detection wavelength 254 nm. The retention time of tolvaptan was found to be 2.59 min with linearity in the concentration range from 37.5 – 225.0 µg/mL, respectively. The mean percentage recovery of tolvaptan was found to be 98.30 – 101.13 %, respectively. The percent relative standard values were less than 2.0 at all the levels and indicates a satisfactory accuracy and precision. The robustness of the method found to meet the acceptance criteria. The stress study against qualified working standard of Tolvaptan, indicated that the developed HPLC method was stability- indicating, conducted as per ICH requirements. The developed method can be handy in the quality control of bulk and pharmaceutical dosage forms.

scholarly journals DETERMINATION OF PINAVERIUM BROMIDE IN PHARMACEUTICAL DOSAGE FORMS BY A VALIDATED STABILITY-INDICATING LC METHOD

2017 ◽  
Vol 1 (1) ◽  
pp. 38-43
Author(s):  
Maximiliano Da Silva Sangoi ◽  
Anna Karolina Mouzer da Silva Machado ◽  
Lorena Coimbra Florindo ◽  
Brenda Rocha Gonçalves ◽  
Vítor Todeschini
Keyword(s):  
Reversed Phase ◽  
Mean Value ◽  
Dosage Forms ◽  
Array Detector ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Photodiode Array Detector ◽  
Relative Standard ◽  
Pinaverium Bromide

A reversed-phase liquid chromatography (LC) method is validated for the determination of pinaverium bromide (PB) in pharmaceutical dosage forms. The LC method is carried out on a reversed-phase monolithic C18 column (100 x 4.6 mm i.d.), maintained at 45 ºC. The mobile phase consisted of acetonitrile and a solution of triethylamine 0.3% pH 5.0 (50:50; v/v), run at a flow rate of 2.0 mL/min, with photodiode array detector set at 213 nm. The chromatographic separation is obtained with PB retention time of 3.4 min, and it is linear in the range of 5-100 μg/mL (r2 = 0.9991). The limits of detection and quantitation are 1.41 and 4.70 μg/mL, respectively. The specificity and stability-indicating capability of the method are proven through degradation studies, which also showed that there is no interference of the formulation excipients, showing that peak is free from any coeluting peak. The method showed adequate precision, with a relative standard deviation values lower than 1.38%. Excellent values of accuracy were also obtained, with a mean value of 100.68%. Experimental design is used during validation to calculate and prove method robustness. The proposed LC method is applied for the analysis of the PB pharmaceutical dosage forms, contributing to improve the quality control and to assure the therapeutic efficacy.

Determination of dronedarone in the pharmaceutical dosage form by a stability-indicating micellar electrokinetic chromatography method

2013 ◽  
Vol 5 (12) ◽  
pp. 3106 ◽  
Author(s):  
Ana Isa Pedroso Marcolino ◽  
Maximiliano S. Sangoi ◽  
Martin Steppe ◽  
Andréa Inês Horn Adams ◽  
Clarice Madalena Bueno Rolim
Keyword(s):  
Dosage Form ◽  
Micellar Electrokinetic Chromatography ◽  
Electrokinetic Chromatography ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating

scholarly journals Development and Validation of Stability Indicating Reverse Phase High Performace Liquid Chromatography Method for the Determination of Umeclidinium and Vilanterol in Pharmaceutical Dosage Form

2021 ◽  
pp. 208-219
Author(s):  
Ahsaana Hamsa ◽  
K. Praseetha ◽  
K. P. Dijin Raj ◽  
T. V. Ashira ◽  
O. V. Athira ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Form ◽  
Relative Standard ◽  
Validation Parameters ◽  
The Stability

A Sensitive, fast, linear and accurate liquid chromatography technique was developed for the simultaneous determination of Umeclidinium and Vilanterol in Powder dosage form. The estimation was carried out using Phenomenex C18 column (150 × 4.6 mm, 5μ) with ammonium acetate: acetonitrile taken in the ratio 60:40 as mobile phase and pumped at a flow rate of 0.9 ml/min at 300C. Detection wavelength selected was 245 nm. Retention times of Umeclidinium and Vilanterol were found to be 2.219 min and 2.794 min. The method was validated in terms of linearity, precision, accuracy, limit of detection, limit of quantification as per International council for harmonization guidelines. Degradation studies performed indicated the stability of the drug. All of these analytical validation parameters were evaluated, and the percent relative standard deviations were calculated, indicating the method's suitability for determination of Umeclidinium and Vilanterol in pharmaceutical dosage form.

scholarly journals Development & Validation of RP-HPLC Method for the Estimation of Doravirine in Bulk and Pharmaceutical Dosage Form

2021 ◽  
pp. 26-31
Author(s):  
A. Suneetha ◽  
G. I. Priyadarshini ◽  
V. Mounika ◽  
G. Aparna
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
Potassium Dihydrogen Phosphate ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Calibration Plot ◽  
Dihydrogen Phosphate ◽  
Pharmaceutical Dosage Form ◽  
Relative Standard

A simple, accurate, rapid and precise isocratic reversed phase high-performance liquid chromatographic method has been developed and validated for determination of Doravirine in tablets. The chromatographic separation was carried out on Dionex C18 (250 x 4.6mm, 5µ) with a mixture of methanol: 0.05M potassium dihydrogen phosphate (40:60%v/v) as a mobile phase at a flow rate of 1.5 mL/min. UV detection was performed at 306 nm. The retention time was 5.24 min for Doravirine. Calibration plot was linear (r2=0.999) over the concentration range of 200-600 µg/mL. The method was validated for accuracy, precision, specificity, linearity, robustness, LOD and LOQ. The proposed method was successfully used for quantitative analysis of tablets. No interference from any component of pharmaceutical dosage form was observed. Validation studies revealed that method is specific, rapid, reliable, and reproducible. The high recovery and low relative standard deviation confirm the suitability of the method for routine determination of Doravirine in bulk and tablet dosage form.

scholarly journals Development and validation of RP-HPLC method for estimation of Vildagliptin from table dosage form

2012 ◽  
Vol 1 (1) ◽  
Author(s):  
Aparajita Malakar ◽  
Bishwajit Bokshi ◽  
Dilruba Nasrin
Keyword(s):  
Dosage Form ◽  
Limit Of Detection ◽  
Phase 1 ◽  
Ammonium Hydroxide ◽  
Reversed Phase ◽  
Hplc Method ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Form ◽  
Limit Of Quantitation

A new simple, specific, precise and accurate reversed-phase liquid chromatography method has been developed for the determination of Vildagliptin (VLG) in pharmaceutical dosage form. The separation was achieved on a Xterra® Waters C18 column (150mm×4.6mm, 5?m) using mobile phase consisting of a mixture of aqueous phase (1 ml of 25% ammonium hydroxide was dissolved in 1000 ml of water for chromatography, pH of the solution was adjusted to the value of 9.5 using a 50% solution of phosphoric acid) and organic phase (methanol) in the ratio of 60:40 v/v at a flow rate of 1.0 ml/min. Detection was carried out at 210nm. The retention time of Vildagliptin was found to be 6.3 min. The calibration curve was found linear between 5- 200?g/ml (r2 = 0.9997). Limit of detection and limit of quantitation were 1.47 and 4.90 ?g/mL, respectively. The percentage recoveries of Vildagliptin were found to be in the range of 99.11-100.62%. The method was validated in accordance with International Conference on Harmonization acceptance criteria for specificity, linearity, precision, accuracy, robustness and system suitability. The excipients did not interfere in the determination of VLG. The proposed method was successfully applied for the quantitative analysis of VLG in tablet dosage form, which will help to improve quality control. DOI: http://dx.doi.org/10.3329/ijpls.v1i1.12947 International Journal of Pharmaceutical and Life Sciences Vol.1(1) 2012

A Validated Stability-Indicating RP-LC Method for the Simultaneous Determination of Amlodipine and Perindopril in Tablet Dosage Form and Their Stress Degradation Behavior Under ICH-Recommended Stress Conditions

2013 ◽  
Vol 96 (4) ◽  
pp. 751-757 ◽  
Author(s):  
Mehmet Gumustas ◽  
Sibel A Ozkan
Keyword(s):  
Simultaneous Determination ◽  
Mobile Phase ◽  
Dosage Form ◽  
Degradation Products ◽  
Stress Conditions ◽  
Assay Method ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Tablet Dosage

Abstract A stability-indicating RP-LC assay method was developed for the simultaneous determination of the cardiovascular drugs amlodipine and perindopril in the presence of degradation products generated from forced decomposition studies. The developed method is applicable for the determination of related substances in bulk drugs and simultaneous assay in a tablet pharmaceutical dosage form. Separation of the drugs and their degradation products was obtained using an RP Waters Spherisorb ODS1 column (250 × 4.6 mm id, 5 μm particle size) with the mobile phase acetonitrile–water (30 + 70, v/v) containing 15 mM phosphoric acid. The pH of the mobile phase was adjusted to 5.0. A flow rate of 1.2 mL/min was used for the separations, with detection at 215 nm. The chromatographic separation was performed at a column temperature of 45°C. Atenolol was chosen as the internal standard. Amlodipine and perindopril were exposed to thermal, photolytic, hydrolytic, and oxidative stress conditions, and the stressed samples were analyzed by the proposed method. Degradation studies showed that both compounds were degraded under these stress conditions. The method was found to be stability-indicating and can be used for the routine analysis of amlodipine and perindopril in the studied combined tablet dosage form.

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