Stability-indicating thin-layer chromatographic method for determination of darunavir in complex darunavir–β-cyclodextrin in the presence of its degradation products

2014 ◽  
Vol 6 (11) ◽  
pp. 3689-3693 ◽  
Author(s):  
Ana Carolina Kogawa ◽  
Jaqueline Nakau Mendonça ◽  
Norberto Peporine Lopes ◽  
Hérida Regina Nunes Salgado
Keyword(s):  
Thin Layer ◽  
Chromatographic Method ◽  
Degradation Products ◽  
Stability Indicating

A method was developed to identify degradation products of the complex darunavir–β-cyclodextrin.

scholarly journals Validated Stability Indicating HPTLC Method for the Determination of Dutasteride in Pharmaceutical Dosage Forms

2011 ◽  
Vol 2011 ◽  
pp. 1-5 ◽  
Author(s):  
Dipti B. Patel ◽  
Natubhai J. Patel ◽  
Sejal K. Patel ◽  
Paresh U. Patel
Keyword(s):  
Thin Layer ◽  
Chromatographic Method ◽  
Degradation Products ◽  
Linear Regression Analysis ◽  
Solvent System ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Wet Heat ◽  
Pure Drug

This paper describes simple, sensitive, precise, specific, and stability-indicating high-performance thin-layer chromatographic method for the determination of dutasteride (DUTA) in bulk and tablet formulation. Validation was carried out in compliance with International Conference on Harmonization guidelines. The thin-layer chromatographic method employed aluminium plates precoated with silica gel G60F254 as stationary phase. The solvent system consisted of toluene/methanol/triethylamine (9 : 2 : 1, v/v/v). This solvent system was found to give compact spots for dutasteride with value 0.71 ± 0.01. Densitometric analysis of DUTA was carried out in the absorbance mode at 274 nm. Linear regression analysis showed good linearity () with respect to peak area in the concentration range of 200–3000 ng per spot. The method was validated for precision, accuracy, specificity, and robustness. Pure drug was subjected to acid and alkali hydrolysis, oxidation, photo degradation, dry heat and wet heat treatment. The drug underwent degradation under acidic, basic, oxidative, and wet heat conditions. The degraded products were well separated from the pure drug. Statistical analysis proved that the method is reproducible and selective for estimation of DUTA in bulk and tablets. As the method could effectively separate the drugs from their degradation products, it can be employed as a stability indicating method.

scholarly journals New Salting Out Stability-Indicating and Kinetic Thin Layer Chromatographic Method for Determination of Glimepiride and Metformin HCl Binary Mixture

2015 ◽  
Vol 53 (9) ◽  
pp. 1603-1610 ◽  
Author(s):  
Yahya Abduh Salim Mohamed ◽  
Abdel Maaboud Ismail Mohamed ◽  
Fardous Abdel-Fattah Mohamed ◽  
Sameh Abdel-Raouf Ahmed
Keyword(s):  
Binary Mixture ◽  
Thin Layer ◽  
Chromatographic Method ◽  
Salting Out ◽  
Stability Indicating ◽  
Metformin Hcl

scholarly journals Validated Stability – Indicating Methods for Determination of Sofosbuvir by UPLC and HPTLC in Pure Form and Tablet Dosage Forms

2019 ◽  
pp. 1-13
Author(s):  
Sawsan A. Abdel-Razeq ◽  
Zeinab Adel Nasr ◽  
Noha S. Said
Keyword(s):  
Liquid Chromatography ◽  
Thin Layer ◽  
High Performance ◽  
Good Accuracy ◽  
Degradation Products ◽  
Dosage Forms ◽  
Stability Indicating ◽  
Accuracy And Precision ◽  
Tablet Dosage

Aims: Two simple and sensitive stability- indicating methods were developed and validated for the quantitative determination of sofosbuvir in presence of its degradation products. Study Design: Ultra high performance liquid chromatography (UPLC), High performance thin layer chromatography (HPTLC) are developed for determination of sofosbuvir in presence of its degradation products, laboratory-prepared mixtures and in tablet dosage forms. Place and Duration of Study: Analytical Chemistry Department, Faculty of Pharmacy (Girls), Al-Azhar University, between August 2018 and March 2019. Methodology: Two simple and sensitive stability- indicating methods were developed and validated for the quantitative determination of Sofosbuvir in presence of its degradation products. The first method was an Ultra Performance Liquid Chromatography (UPLC) method, in which efficient separation was carried out on phenomenex kinetex 2.6 μm C18 100 A column using a mobile phase consisting of filtered and degassed mixture of 0.1% ortho-phosphoric acid in water and methanol with the ratio of (40:60% v/v) adjusted to pH 3.5, at a flow rate of 1 mL min-1 and UV detection at 260 nm at ambient temperature. The second method is a high performance- thin layer chromatographic one (HPTLC) in which chromatographic separation was performed on silica gel 60 F254 plates, with methanol – chloroform – ammonia (2.5: 6: 1.5 % v/v/v) as a developing system followed by densitometric determination at 261 nm. Sofosbuvir was subjected to stress conditions including alkaline, acidic and oxidative degradation. Results: Beer’s law was obeyed over the range of 1-20 μg mL–1 for UPLC and 2-12 μg / spot for HPTC with good accuracy and precision using the two procedures, respectively. Results obtained was statistically analysed and found to be in accordance with those given by the reported method. Conclusion: The proposed methods were successfully applied for the determination of sofosbuvir in bulk powder, laboratory prepared mixtures and pharmaceutical dosage form with good accuracy and precision. The methods were validated according to ICH guidelines. The results obtained were compared with those of the reported method and were found to be in good agreement.

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