scholarly journals Four new degradation products of doxorubicin: An application of forced degradation study and hyphenated chromatographic techniques

2015 ◽  
Vol 5 (5) ◽  
pp. 285-295 ◽  
Author(s):  
Dheeraj Kaushik ◽  
Gulshan Bansal
Keyword(s):  
Degradation Products ◽  
Forced Degradation ◽  
Degradation Study ◽  
Chromatographic Techniques

Synthesis and Characterization of Potential and Degraded Impurities of Regadenoson

2020 ◽  
Vol 16 (8) ◽  
pp. 1130-1139
Author(s):  
Singaram Sathiyanarayanan ◽  
Chidambaram Subramanian Venkatesan ◽  
Senthamaraikannan Kabilan
Keyword(s):  
Mass Spectra ◽  
Degradation Products ◽  
Hplc Method ◽  
Forced Degradation ◽  
Spectroscopic Techniques ◽  
A2a Adenosine Receptor ◽  
Degradation Study ◽  
Related Substances ◽  
Adenosine Receptor Agonist

Background: Regadenoson is an A2A adenosine receptor agonist that is a coronary vasodilator and commonly used as a pharmacologic cardiac stressing agents. Methods: HPLC method was used for the analysis of related substances. The degraded impurities during the process were isolated and characterized by IR, Mass and NMR spectral analysis. Results: Forced degradation study of regadenoson under conditions of hydrolysis (neutral, acidic and alkaline) and oxidations suggested in the ICH Q1A(R2) was accomplished. The drug showed significant degradation under all the above conditions. On the whole, five novel degradation products were found under diverse conditions along with process related impurities which were not reported earlier. Conclusion: All the degradation products were well characterized by using advanced spectroscopic techniques like IR, 1H NMR, 13C NMR and Mass spectra. The identification of these impurities will be productive for the quality control during the production and stability behavior of the regadenoson drug substance.

scholarly journals Determination of Rosuvastatin in the Presence of Its Degradation Products by a Stability-Indicating LC Method

2005 ◽  
Vol 88 (4) ◽  
pp. 1142-1147 ◽  
Author(s):  
Tushar N Mehta ◽  
Atul K Patel ◽  
Gopal M Kulkarni ◽  
Gunta Suubbaiah
Keyword(s):  
Degradation Products ◽  
Stability Study ◽  
Tablet Formulation ◽  
Assay Method ◽  
Forced Degradation ◽  
Degradation Study ◽  
Stability Indicating ◽  
Degraded Samples ◽  
Accelerated Stability

Abstract A forced degradation study was successfully applied for the development of a stability-indicating assay method for determination of rosuvastatin Ca in the presence of its degradation products. The method was developed and optimized by analyzing the forcefully degraded samples. Degradation of the drug was done at various pH values. Moreover, the drug was degraded under oxidative, photolytic, and thermal stress conditions. Mass balance between assay values of degraded samples and generated impurities was found to be satisfactory. The proposed method was able to resolve all of the possible degradation products formed during the stress study. The developed method was successfully applied for an accelerated stability study of the tablet formulation. The major impurities generated during the accelerated stability study of the tablet formulation were matches with those of the forced degradation study. The developed method was validated for determination of rosuvastatin Ca, and the method was found to be equally applicable to study the impurities formed during routine and forced degradation of rosuvastatin Ca.

Characterization of stress degradation products of blonanserin by UPLC-QTOF-tandem mass spectrometry

RSC Advances ◽  
2015 ◽  
Vol 5 (85) ◽  
pp. 69273-69288 ◽  
Author(s):  
Pradipbhai D. Kalariya ◽  
Prinesh N. Patel ◽  
Mahesh Sharma ◽  
Prabha Garg ◽  
R. Srinivas ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
High Resolution ◽  
Tandem Mass Spectrometry ◽  
Degradation Products ◽  
Structural Elucidation ◽  
Forced Degradation ◽  
Tandem Mass ◽  
Degradation Study ◽  
Stress Degradation

Forced degradation study of blonanserin and structural elucidation of its degradation products was performed using high resolution tandem mass spectrometry.

Characterization of the degradation products of bambuterol using LCMS-QTOF and NMR

2015 ◽  
Vol 7 (18) ◽  
pp. 7659-7673 ◽  
Author(s):  
A. Abiramasundari ◽  
V. Sudarsanam ◽  
Kamala K. Vasu
Keyword(s):  
Degradation Products ◽  
Forced Degradation ◽  
Degradation Study ◽  
Ich Guidelines ◽  
Mechanisms Of Formation

A systematic forced degradation study of bambuterol was carried out according to ICH guidelines. Twelve degradation products of bambuterol were identified and characterized. Plausible mechanisms of formation of the degradation products are discussed.

scholarly journals Identification of degradation impurity of TGR5 receptor agonist-ZY12201 by LC–MS technique during force degradation study

2021 ◽  
Vol 3 (6) ◽  
Author(s):  
Chandrakant Sojitra ◽  
Chintan Dholakia ◽  
Padmaja Sudhakar ◽  
Kumar K. Singh ◽  
Sameer Agarwal
Keyword(s):  
Degradation Products ◽  
Oxidative Degradation ◽  
Active Pharmaceutical Ingredient ◽  
Storage Conditions ◽  
Receptor Activation ◽  
Degradation Pathway ◽  
Forced Degradation ◽  
Degradation Study ◽  
Glucagon Like Peptide 1 ◽  
Orally Bioavailable

AbstractForced degradation study is a systemic characterization of degradation products of active pharmaceutical ingredient (API) at conditions which posses more harsh environment that accelerates degradation of API. Forced degradation and stability studies would be useful in selection of proper, packaging material and storage conditions of the API. These are also useful to demonstrate degradation pathways and degradation products of the API and further characterisation of the degradation products using mass spectrometry. TGR5 is a G protein-coupled receptor, activation of which promotes secretion of glucagon-like peptide-1 (GLP-1) and modulates insulin secretion. The potent and orally bioavailable TGR5 agonist, ZY12201, shows activation of TGR5 which increase secretion of GLP-1 and help in lowering blood glucose level in animal models. Hence it is necessary to establish and study degradation pathway and stability of API for better handling and regulatory approval. Force degradation studies of ZY12201 have shown presence of one oxidative impurity during oxidative degradation in HPLC analysis. The oxidized product is further characterized by LC–MS to elucidate structure of impurity and characterize its degradation pathway.

scholarly journals FORCED DEGRADATION STUDY OF STATINS: A REVIEW

2018 ◽  
Vol 10 (6) ◽  
pp. 38
Author(s):  
Rini Yulianita ◽  
Iyan Sopyan ◽  
Muchtaridi Muchtaridi
Keyword(s):  
Degradation Products ◽  
Storage Conditions ◽  
Lipid Lowering ◽  
Forced Degradation ◽  
Degradation Study ◽  
Drug Degradation ◽  
Drug Products ◽  
Drug Substances ◽  
Accelerated Stability ◽  
Forced Degradation Studies

Forced degradation study is the degradation of new drug substances and drug products in more severe conditions than accelerated conditions. Forced degradation study were conducted to demonstrate the specificity of stability-indicating methods, providing insight into degradation pathways and drug degradation products, assisting in the elucidation of degradation product structures, identifying degradation products that could be spontaneously generated during storage and use of drugs and to facilitate improvement in manufacturing process and formulation corresponding with accelerated stability studies. Statins, a class of lipid-lowering medications, are the most widely prescribed drugs and an example of an unstable drug. Statins are susceptible to hydrolysis in the presence of high temperatures and humidity. Therefore, the review discusses various studies of forced degradation studies in six statins drug (atorvastatin, fluvastatin, pitavastatin, pravastatin, rosuvastatin, and simvastatin) to describe the drug's intrinsic stability thus it can assist the selection of formulations and packaging as well as proper storage conditions.

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.

scholarly journals Optimization of a forced degradation study of atorvastatin employing an experimental design approach

2018 ◽  
Vol 37 (2) ◽  
Author(s):  
Maja Hadzieva Gigovska ◽  
Ana Petkovska ◽  
Jelena Acevska ◽  
Natalija Nakov ◽  
Blagica Manchevska ◽  
...  
Keyword(s):  
Experimental Design ◽  
Ion Trap ◽  
Degradation Products ◽  
Forced Degradation ◽  
Experimental Conditions ◽  
Liquid Chromatograph ◽  
Degradation Study ◽  
Mobile Phases ◽  
Forced Degradation Studies ◽  
Full Factorial

This study involved the optimization of experimental conditions for the forced degradation of atorvastatin employing the experimental design (DoE) approach, as a scientific multifactorial strategy. Using 2n full factorial design, stress conditions of oxidative, hydrolytic and thermal degradation were optimized to obtain a targeted level of atorvastatin degradation. Atorvastatin and all related and degradation products were separated on Poroshell 120 EC C18 50 ´ 3.0 mm 2.7 μm, using 10 mM ammonium formate and acetonitrile as mobile phases in the gradient mode. The impurity structures were confirmed by the direct hyphenation of a liquid chromatograph to an ion trap mass spectrometer with a heated electrospray ionization interface.This study highlights the multifold benefits of implementing the DoE concept, which provides a better understanding of the significant factors responsible for degradation and ensures a successful way to achieve degradation, thereby replacing the trial and error approach used in conventional forced degradation studies.

Sign in / Sign up

Export Citation Format

Share Document