scholarly journals Evaluation of physicochemical stability and degradation kinetics of bedaquiline in hydrolytic solutions of different pH

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
S. J. Rajput ◽  
P. J. Vanavi
Keyword(s):  
High Performance ◽  
Degradation Kinetics ◽  
Regression Line ◽  
Reversed Phase ◽  
Stability Study ◽  
Enthalpy Of Reaction ◽  
Formulation Development ◽  
Kinetics Parameters ◽  
Degradation Kinetic ◽  
Key Aspects

Abstract Background Tuberculosis is an infection that has high mortality rate in human as well as in animals if it remains unattained for long time. Scientists are always desirous to discover new molecules against Mycobacterium tuberculosis; one of them is bedaquiline which was recently approved to treat multidrug resistance TB. During the clinical study of new molecule stability and impurity are the key aspects to develop formulation. Stability issues in bulk drug are dangerous to drug safety and needs careful attention in formulation development. Bedaquiline stability study was completed with reversed-phase high-performance liquid chromatography (HPLC) and utilized in degradation kinetic study of bedaquiline in aqueous condition under different pH, temperature, and concentrations of degradant. Results Linearity was obtained in 50.0-250.0μg/ml, correlation coefficient, and regression line equation were 0.998 and Y=18528x + 7E+06 respectively. Intraday, inter day precision, and repeatability RSD were less than 2.0%. Average recovery in accuracy study was more than 98.0% showed that good recovery was obtained. Degradation kinetics parameters like activation energy (Ea), half-life (t50), rate constant (k), and shelf life (t90) were calculated under different condition for bedaquiline. Entropy and enthalpy of reaction was studied to gather knowledge about energy of system. Conclusion The result explained that bedaquiline degradation was pH-dependant, as increase in concentration of degradant and temperature, there was increase in degradation rate of bedaquiline. Bedaquiline was stable in neutral aqueous condition and at lower temperatures, shows that drug is hydrophobic in nature. Kinetic data showed that bedaquiline followed first order kinetics in acidic and alkaline pH.

Development and Validation of Stability Indicating High-Performance Thin-Layer Chromatographic (HPTLC) Method for Quantification of Asiaticoside from Centella asiatica L. and its Marketed Formulation

2019 ◽  
Vol 102 (4) ◽  
pp. 1014-1020
Author(s):  
Lisa J Patel ◽  
Manan A Raval ◽  
Samir G Patel ◽  
Archita J Patel
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Degradation Kinetics ◽  
Centella Asiatica ◽  
Stability Study ◽  
Cns Disorders ◽  
Marker Compound ◽  
Plant Powders ◽  
Development And Validation ◽  
Hptlc Method

Abstract Background: Ayurvedic medicines help in healing disease with fewer undesirable effects in comparison with an allopathic system of medicine to treat central nervous system (CNS) disorders, as the latter is more expensive. Centella asiatica L. is often used in Ayurvedic formulations for the treatment of CNS disorders. Objective: A stability test using an HPTLC method for the estimation of an important marker asiaticoside (ASI) from C. asiatica powder and marketed formulation was developed. Methods: The marker compound ASI from plant powders and marketed formulations were resolved using toluene–ethyl acetate–methanol–glacial acetic acid (2+7+3+1, v/v/v/v) as the mobile phase and then was derivatized. The plant powder and marketed formulation were also subjected to stability studies. Results: The Rf value of ASI was found in range of 0.43–0.47 for the standard ASI, plant powder, and marketed formulation. It was found that the plant powder and formulation exhibited first-order degradation kinetics. Conclusions: The contents of ASI in the formulation (Churna) and its flow characters reduced at the end of the 6 months during an accelerated stability study. The developed method can be used to quantify ASI in the presence of its degradation products. Highlights: The developed method helps in determining batch to batch variation in the content of ASI in herbal formulations.

scholarly journals Development and Validation of an HPLC Method to Quantify Camptothecin in Polymeric Nanocapsule Suspensions

2008 ◽  
Vol 91 (3) ◽  
pp. 551-556 ◽  
Author(s):  
Andra Granada ◽  
Fabio S Murakami ◽  
Tatiane Sartori ◽  
Elenara Lemos-Senna ◽  
Marcos A S Silva
Keyword(s):  
High Performance ◽  
Early Stage ◽  
Current Method ◽  
Entrapment Efficiency ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Calibration Graph ◽  
Formulation Development ◽  
Relative Standard ◽  
Limit Of Quantitation

Abstract A simple, rapid, and sensitive reversed-phase column high-performance liquid chromatographic method was developed and validated to quantify camptothecin (CPT) in polymeric nanocapsule suspensions. The chromatographic separation was performed on a Supelcosil LC-18 column (15 cm 4.6 mm id, 5 m) using a mobile phase consisting of methanol10 mM KH2PO4 (60 + 40, v/v; pH 2.8) at a flow rate of 1.0 mL/min and ultraviolet detection at 254 nm. The calibration graph was linear from 0.5 to 3.0 g/mL with a correlation coefficient of 0.9979, and the limit of quantitation was 0.35 g/mL. The assay recovery ranged from 97.3 to 105.0. The intraday and interday relative standard deviation values were <5.0. The validation results confirmed that the developed method is specific, linear, accurate, and precise for its intended use. The current method was successfully applied to the evaluation of CPT entrapment efficiency and drug content in polymeric nanocapsule suspensions during the early stage of formulation development.

scholarly journals Stability-Indicating UHPLC Method for the Determination of Desvenlafaxine: Application to Degradation Kinetics

2021 ◽  
Vol 20 (2) ◽  
pp. 167-176
Author(s):  
Halima Akter ◽  
Md Mahbubul Alam ◽  
Md Rezoan Rabbi ◽  
Abu Shara Shamsur Rouf
Keyword(s):  
High Performance ◽  
Uv Light ◽  
Degradation Kinetics ◽  
Reversed Phase ◽  
Drug Substance ◽  
Forced Degradation ◽  
Order Kinetic ◽  
Great Resistance ◽  
Photolytic Degradation ◽  
Recommended Guidelines

This study was aimed to investigate the degradation behavior and physicochemical stability of desvenlafaxine using reversed-phase ultra-high-performance liquid chromatography (RP-UHPLC) system. The chromatogram was developed on Eclipse XDB-C8 column (150 x 4.6 mm, 5μm). The eluents were monitored through a photo diode array plus (PDA+) detector at 210 nm using an isocratic method with a flow rate of 1.5 ml/min. Mobile phase composition was 30:70 v/v mixture of 0.1 % trifluoroacetic acid (TFA) in water and methanol. Forced degradation studies were performed on drug substance of desvenlafaxine as per International Conference on Harmonization (ICH) prescribed stressed conditions (Q1A(R2) and Q1B) using hydrolytic (acidic, basic, and neutral), oxidative and photolytic methods. The drug substance was found highly labile to acidic (0.5 N hydrochloric acid, 18.65 % degradation in 2 hours at 70°C), basic (1.0 N sodium hydroxide, 11.01 % degradation in 12 hours at 70°C) and oxidative (3 % hydrogen peroxide, 17.05 % degradation in 2 hours at 50°C) stressed conditions, but a great resistance was observed towards dry heat (maximum degradation 0.27 % in 10 days from ambient to higher temperature, 80°C), moist heat (maximum degradation 0.25 % in 2 hours at 80°C and 75 % relative humidity) as well as in photolytic degradation (maximum degradation 0.23 % in 10 days at UV light of 315 - 400 nm). A pseudo-first order kinetic was followed in acidic, basic and peroxide degradation methods which paved a way to calculate the half-life of the drug substance desvenlafaxine under ICH mentioned stressed conditions. The results were also statistically analyzed and the % RSD values were compared with recommended guidelines. Dhaka Univ. J. Pharm. Sci. 20(2): 167-176, 2021 (December)

scholarly journals Stability Study of Etoricoxib a Selective Cyclooxygenase-2 Inhibitor by a New Single and Rapid Reversed Phase HPLC Method

Symmetry ◽  
2018 ◽  
Vol 10 (7) ◽  
pp. 288
Author(s):  
Muhammad Alzweiri ◽  
Mariam Sallam ◽  
Walid Al-Zyoud ◽  
Khaled Aiedeh
Keyword(s):  
Liquid Chromatography ◽  
High Performance ◽  
Internal Standard ◽  
Ultra Performance Liquid Chromatography ◽  
Reversed Phase ◽  
Stability Study ◽  
Cyclooxygenase 2 ◽  
Crystal Formation ◽  
Acute Gout ◽  
Cox 2

Cyclooxygenase-2 (COX-2) is an enzyme responsible for inflammation and pain. Etoricoxib is the most recent selective (COX-2) inhibitor that has a higher COX-2 selectivity than the other COX-2-selective nonsteroidal anti-inflammatory drugs (NSAIDs), which significantly improves its gastric safety profile. The current therapeutic indications of etoricoxib includes the treatment of several painful conditions, such as osteoarthritis, acute gout, ankylosing spondylitis, and rheumatoid arthritis. To the best of found knowledge, no decent method has been reported that can be used for the routine determination of etoricoxib and additives in pharmaceutical suspensions by a single, rapid and cost-effective run of HPLC, using an UV-Vis detector. Earlier reported methods, such as liquid chromatography-mass spectrometry (LC-MS), high performance thin layer chromatography (HPTLC), capillary zone electrophoresis, and ultra performance liquid chromatography (UPLC), are all tedious and time consuming. A reversed phase high performance liquid chromatography (RP-HPLC) was used as a first reported single run method to achieve developed and validated simultaneous determination for sodium saccharin, vanillin, methyl paraben, etoricoxib, and butyl paraben, in prepared oral suspensions of etoricoxib. Reversed phase column of octadecylsilane (ODS) C18 with isocratic mobile phase containing methanol, and phosphate buffer of pH 6 in a ratio of 70:30 (v/v). Celecoxib is used as an internal standard at a detection wavelength of 215 nm. This method separates the analytes in a total running time less than 13 min. Linearity is obtained in the calibration curve for all analytes with a R2 value of > 0.999. Furthermore, beta-cyclodextrin (β-CD) and 2-hydroxypropyl-β-cyclodextrin (HP-β-CD) were added, either alone or combined, to prevent the crystal formation, and any unpleasant taste of etoricoxib in oral formulations. After testing both HP-β-CD and β-CD at 3% w/w for each, the results showed that HP-β-CD is more efficient in preventing the crystal formation of etoricoxib in suspensions at room temperature than β-CD is.

Hydrolytic Degradation Kinetic Study of Balofloxacin by Stability Indicating Reversed Phase High Performance Liquid Chromatography Method

2016 ◽  
Vol 7 (1) ◽  
pp. 39-47 ◽  
Author(s):  
Bhavin Pankajbhai Marolia ◽  
Pintu Bhagwanbhai Prajapati ◽  
Kunjan Bharatbhai Bodiwala ◽  
Megha Pravinkumar Vaghela ◽  
Shailesh Amritlal Shah ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Kinetic Study ◽  
High Performance ◽  
Hydrolytic Degradation ◽  
Reversed Phase ◽  
Chromatography Method ◽  
Degradation Kinetic ◽  
Stability Indicating ◽  
Liquid Chromatography Method

scholarly journals The stability and degradation kinetics of acetylsalicylic acid in different organic solutions revisited – an UHPLC–ESI-QTOF spectrometry study

2016 ◽  
Vol 29 (1) ◽  
pp. 39-41 ◽  
Author(s):  
Robert Skibinski ◽  
Lukasz Komsta
Keyword(s):  
Mass Spectrometry ◽  
Salicylic Acid ◽  
Acetylsalicylic Acid ◽  
High Performance ◽  
Degradation Kinetics ◽  
Water Solution ◽  
Stability Study ◽  
Initial Concentration ◽  
The Stability ◽  
Organic Solutions

Abstract Ultra high performance liquid chromatography (UHPLC), coupled with accurate quadrupole-time-of-flight (Q-TOF) mass spectrometry, was used for the stability study of acetylsalicylic acid within a variety of different organic solutions: methanol, ethanol, propan-2-ol, acetonitrile, tetrahydrofuran and 1,4-dioxane. With the use of gradient elution chromatography and mass spectrometry detection in negative ionization, MS and MS/MS spectra were recorded simultaneously. In addition, quantitative, as well as qualitative analysis was performed during one assay. The stability of acetylsalicylic acid in such solutions was tested at room temperature, in a 12h period. In the work, in all cases, only one main degradation product, salicylic acid, was found. What is more, the work revealed that the degradation of aspirin in the tested organic solutions yields apparent second-order kinetics. The study also demonstrated that acetonitrile and 1,4-dioxane turned out to be the most stable solvents, and an above 80% of initial concentration of acetylsalicylic acid was found in this case. Furthermore, the most popular analytical solvents, methanol and ethanol, were found to be very unstable media. Herein, below 40% of initial concentration of acetylsalicylic acid was seen after 12h. The obtained results were also compared with the degradation of acetylsalicylic acid in a water solution. In this situation, only about 25% of the analyzed compound was resolved to salicylic acid in the same time frame.

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