Stability-indicating HPLC method development and structural elucidation of novel degradation products in posaconazole injection by LC–TOF/MS, LC–MS/MS and NMR

Yang, Yidi; Zhu, Xi; Zhang, Fei; Li, Wei; Wu, Ying; Ding, Li

doi:10.1016/j.jpba.2016.03.034

Cited by 13 publications

(3 citation statements)

References 24 publications

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“…Bilastine is reported as a degradation product of Bilastine in the literature also 6,13 . Similar outcomes were revealed about the genesis of N-oxide derivatives under such conditions [19][20][21][22][23][24] .…”

Section: Characterization Of Degradation Products Using Lc-ms/mssupporting

confidence: 69%

Stability Indicating Isocratic HPLC Method for Bilastine and Characterization of Forced Degradation Products by LC-MS/MS

Patel

Pasha²

2022

Int J Life Sci Pharm Res

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The present study aims to develop and validate a simple, precise, accurate, stability indicating and isocratic reversephase high-performance liquid chromatography (RP-HPLC) method for estimating Bilastine in bulk and synthetic mixture. Bilastine from its degradation products were well separated and estimated on Discovery C8 column (250 mm x 4.6 mm, 5μm) using methanol: 0.1% ortho-phosphoric acid (55:45 %v/v) as a mobile phase and detection was performed at 276 nm by PDA detector. The degradation of Bilastine was studied under different ICH recommended stress conditions. The developed stability-indicating method was validated for system suitability, linearity, accuracy, precision, robustness, detection limit and quantitation as per ICH guidelines. The method was linear over 25-150 μg/ml. Mathematically computed Limit of Detection and Limit of Quantitation were found to be 0.19μg/ml and 0.57μg/ml, respectively. It was discovered that Bilastine degrades under acid and oxidation conditions. By using LC-MS/MS analysis, the structure of Bilastine breakdown products created amid acidic and oxidative settings was elucidated. A complete fragmentation pathway of Bilastine was established to elucidate the degradation products' structures using LC–MS/MS. The elemental concentrations of oxidation products and their fragmentation products were studied using the acquired mass values. The overall data was utilized to describe the degradation of products and their fragmentation process. The developed method can be used for routine analysis of Bilastine in dosage form as it can estimate of Bilastine in presence of excipients and degradation products.

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Section: Characterization Of Degradation Products Using Lc-ms/mssupporting

confidence: 69%

Stability Indicating Isocratic HPLC Method for Bilastine and Characterization of Forced Degradation Products by LC-MS/MS

Patel

Pasha²

2022

Int J Life Sci Pharm Res

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“…Structural characterization provides information related to the characteristics or origin of degradation impurities and their genotoxic potential, drug degradation pathway, mechanism, and chemistry (Foti et al, 2013; Singh et al, 2012). LC–MS is a well‐known technique for the characterization of DPs or impurities as it provides putative structural information in a short time (Abdel‐Ghany et al, 2015; Pan et al, 2006; Yang et al, 2016). A high‐resolution mass spectrometry (HRMS) system provides an accurate mass of up to four to six decimal places, which determines the exact elemental composition.…”

Section: Introductionmentioning

confidence: 99%

Differential role of potential stressors, underlying degradation mechanism, characterization of degradants using LC–MS/MS, and establishment of a stability‐indicating analytical method for duvelisib

Tapkir,

Sahu,

Rajput

et al. 2023

Biomedical Chromatography

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Duvelisib (DUV) was first approved globally in 2018. An extensive literature search revealed that the differential role of a potential degradation medium in altering the shelf‐life of DUV due to its exposure during storage has not been identified till date. Moreover, its degradation impurities and degradation mechanism are not known. In addition, no analytical method has been reported for the quantification of DUV in the presence of its degradation impurities. Therefore, the aim of this study was to identify the impact of different potential degradation media on the stability of DUV, establish the degradation mechanism, and identify its major degradation impurities. The aim was also to establish a stability‐indicating analytical method for the quantification of DUV in the presence of its degradation impurities. This study is the first to report the structure of degradation impurities and the step‐by‐step degradation mechanism of DUV. This information will be useful for the scientific community and manufacturers in optimizing the formulation parameters and/or storage conditions. The validated method can be employed for analysis of stability study and routine quality control samples of newer DUV formulations in pharmaceutical industries. The identified impurities may serve as impurity standards for specifying their limits in the drug after required qualification studies.

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“…Mechanism and kinetics are two major questions to be addressed in a degradation study. As one of the most powerful analytical tools in study of degradation mechanism, HPLC-MS is known for rapid compound identification with the help of widely used chemical databases [ 3 – 5 ]. In order to perform kinetic modeling in degradation study, both reactant and degradation products should be quantitatively analyzed and HPLC-UV is the dominant technique used [ 6 – 8 ].…”

Section: Introductionmentioning

confidence: 99%

Degradation Kinetics and Mechanism of Lithospermic Acid under Low Oxygen Condition Using Quantitative 1H NMR with HPLC-MS

Pan

Gong

2016

PLoS ONE

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A novel quantitative 1H NMR (Q-NMR) combined with HPLC-MS method has been proposed for investigating the degradation process of traditional Chinese medicine (TCM) components. Through this method, in-situ monitoring of dynamics degradation process of lithospermic acid (LA), one of the popular polyphenolic acids in TCM, was realized under low oxygen condition. Additionally, this methodology was proved to be simple, rapid and specific. Degradation kinetic runs have been carried out to systematically investigate the effects of two key environmental factors, initial pH values and temperatures. Eight main degradation products of LA were detected, seven of which were tentatively structural elucidated with the help of both NMR and LC-MS in this work and salvianolic acid A (Sal A) was the primary degradation product of LA. A possible degradation pathway of LA was proposed, subsequently. The results showed that the degradation of LA followed pseudo-first-order kinetics. The apparent degradation kinetic constants increased as the initial pH value of the phosphate buffer increased. Under the given conditions, the rate constants of overall degradation as a function of temperature obeyed the Arrhenius equation. Our results proved that the Q-NMR combined with HPLC-MS method can be one of the most promising techniques for investigating degradation process of active components in TCM.

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Stability-indicating HPLC method development and structural elucidation of novel degradation products in posaconazole injection by LC–TOF/MS, LC–MS/MS and NMR

Cited by 13 publications

References 24 publications

Stability Indicating Isocratic HPLC Method for Bilastine and Characterization of Forced Degradation Products by LC-MS/MS

Stability Indicating Isocratic HPLC Method for Bilastine and Characterization of Forced Degradation Products by LC-MS/MS

Differential role of potential stressors, underlying degradation mechanism, characterization of degradants using LC–MS/MS, and establishment of a stability‐indicating analytical method for duvelisib

Degradation Kinetics and Mechanism of Lithospermic Acid under Low Oxygen Condition Using Quantitative 1H NMR with HPLC-MS

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