Development of a stability-indicating LC method for determination of a synthetic chalcone derivative in a nanoemulsion dosage form and identification of the main photodegradation product by LC–MS

2012 ◽  
Vol 70 ◽  
pp. 652-656 ◽  
Author(s):  
Cristiane B. Mattos ◽  
Vânia B. Deponti ◽  
Fabiano Barreto ◽  
Cláudia M.O. Simões ◽  
Carla R. Andrighetti-Frohner ◽  
...  
Keyword(s):  
Dosage Form ◽  
Stability Indicating ◽  
Photodegradation Product ◽  
Chalcone Derivative

Stability Indicating Photodiode Array Detector Based Estimation of Dapagliflozin Propanediol Monohydrate in API and Tablet Dosage Form by RP-UPLC

2021 ◽  
pp. 4635-4639
Author(s):  
Ashok B. Patel ◽  
Ekta H. Vaghasiya ◽  
Amit R. Dudhatra ◽  
Amitkumar J. Vyas ◽  
Ajay I. Patel ◽  
...  
Keyword(s):  
Dosage Form ◽  
Active Pharmaceutical Ingredient ◽  
Array Detector ◽  
Column Temperature ◽  
Stability Indicating ◽  
Photodiode Array Detector ◽  
Acceptable Method ◽  
Photodiode Array ◽  
Tablet Dosage

Stability indicating RP-UPLC photo diode array detector based method for determination of Dapagliflozin propanediol monohydrate (DPM) in active pharmaceutical ingredient (API) and in tablet dosage form (5mg dapagliflozin) has been developed and validated on Bridge Ethylene Hybride (BEH) C18 column (50mm × 2.1 mm, 1.7µm). Mobile phase composition was water: acetonitrile (60:40 v/v), flow rate 0.5ml/min and detection carried out at 223nm at column temperature 30ºC. Chromatographic separation achieved within 2 min with retention time 0.77 min. Linearity of the method was found over the concentration range of 25-75µg/ml (R2 = 0.9977). The degradation was carried out in five different stress conditions. The developed method was able to resolve peak of API from all generated peaks. Sufficient degradation was achieved in the range of 5.25 to 12.31%. The peak purity is acceptable, Method validation was performed as per ICH guideline Q2(R1).

VALIDATED STABILITY INDICATING SPECTROSCOPIC METHOD FOR ESTIMATION OF DEGRADATION BEHAVIOUR OF VALSARTAN AND HYDROCHLOROTHIAZIDE IN TABLET FORMULATION

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (11) ◽  
pp. 53-59
Author(s):  
Tukaram M. Kalyankar ◽  
◽  
Shital S. Dange ◽  
Shivraj B. Hambarde ◽  
Shailesh J. Wadher ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Dosage Form ◽  
Spectroscopic Method ◽  
Stress Conditions ◽  
Spectrometric Method ◽  
Degradation Behaviour ◽  
Stability Indicating ◽  
Photolytic Degradation ◽  
Tablet Dosage

A simple, accurate and precise UV spectrometric method has been developed for the simultaneous determination of valsartan and hydrochlorothiazide in tablet dosage form. Spectra of valsartan and hydrochlorothiazide in methanol and water (50:50 V/V) show λ max at 250.0 nm and 271.4 nm, respectively. Valsartan and hydrochlorothiazide are subjected to various stress conditions like acid, alkali, thermal and photolytic degradation. Beer’s law was obeyed in concentration range of 4- 24 µg mL-1 for valsartan and 0.5-3 µg mL-1 for hydrochlorothiazide at their respective wavelengths. The proposed method was successfully applied to tablet dosage form for determination of both drugs. The percentage recovery of valsartan and hydrochlorothiazide were found to be 100.19 % and 99.51 %, respectively. A novel accurate and precise stability indicating spectroscopic method has been developed for estimation of valsartan and hydrochlorothiazide.

scholarly journals Validation of a Stability-Indicating RP-HPLC Method for the Determination of Entecavir in Tablet Dosage Form

2010 ◽  
Vol 93 (2) ◽  
pp. 523-530 ◽  
Author(s):  
Sérgio Luiz Dalmora ◽  
Maximiliano da Silva Sangoi ◽  
Daniele Rubert Nogueira ◽  
Lucélia Magalhães da Silva
Keyword(s):  
Dosage Form ◽  
Potassium Phosphate ◽  
Hplc Method ◽  
Forced Degradation ◽  
Photodiode Array Detection ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Forced Degradation Studies ◽  
Tablet Dosage

Abstract An RP-HPLC method was validated for the determination of entecavir in tablet dosage form. The HPLC method was carried out on a Gemini C18 column (150 4.6 mm id) maintained at 30C. The mobile phase consisted of acetonitrilewater (95 + 5, v/v)/potassium phosphate buffer (0.01 M, pH 4; 9 + 91, v/v) pumped at a flow rate of 1.0 mL/min. Photodiode array detection was at 253 nm. The chromatographic separation was obtained with a retention time of 4.18 min, and the method was linear in the range of 0.5200 g/mL (r2 0.9998). The specificity and stability-indicating capability of the method was proven through forced degradation studies, which also showed that there was no interference of the excipients and an increase of the cytotoxicity only by the basic condition. The accuracy was 101.19, with bias lower than 1.81. The LOD and LOQ were 0.39 and 0.5 g/mL, respectively. Method validation demonstrated acceptable results for precision and robustness. The proposed method was applied for the analysis of tablet formulations, to improve QC and assure therapeutic efficacy.

Development and Validation of Two Robust Stability-Indicating Chromatographic Methods for Determination of Metolazone in Drug Substance and Pharmaceutical Dosage Form in the Presence of Its Degradation Products and Characterization of Main Degradation Products Based on LC-MS

2019 ◽  
Vol 58 (3) ◽  
pp. 251-261
Author(s):  
Hala E Zaazaa ◽  
Rasha Abdel-Ghany ◽  
M Abdelkawy ◽  
Mahmoud Sayed
Keyword(s):  
Dosage Form ◽  
Degradation Products ◽  
Hplc Method ◽  
Drug Substance ◽  
Design Parameters ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Chromatographic Methods ◽  
Hptlc Method

Abstract Two robust and selective stability-indicating chromatographic methods were developed and validated for the determination of metolazone in drug substance and pharmaceutical dosage form in the presence of its degradation products. The HPLC method employed a Kromasil C18 (250 × 4.6,5 μm) column and a mobile phase of acetonitrile: 0.2% orthophosphoric acid (32:68 v/v) at a flow rate 2 mL/min and detection at 238 nm. The separation was performed in HPLC isocratic mode. The robustness of the suggested method was assessed using the Plackett–Burman design, parameters affecting system suitability were established and non-significant intervals for the significant parameters were considered. The HPTLC method employed Nano-SIL-20 UV254 HPTLC plates as adsorbent, ethyl acetate: toluene: acetic acid solution (4:4:0.5, v/v/v), as a developing solvent system and densitometric detection at 238 nm. Metolazone was exposed to different stress conditions, including acid and alkaline hydrolysis and oxidative and photolytic degradation. The main degradation products obtained have been characterized and interpreted based on LC-MS. The linearity of the suggested methods was proved in the concentration range of 20–75 μg/mL for the HPLC method and 100–900 ng/spot for the HPTLC method. The suggested methods were validated according to international conference on harmonization guidelines. These methods were successfully dedicated for the estimation of metolazone in drug substance and pharmaceutical dosage form in the presence of its degradation products. The results of the suggested methods were evaluated and compared statistically with results obtained by an official method without finding any significant difference.

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