Identification and characterization of Prothionamide degradation impurities by mass spectrometry, NMR spectroscopy, and ultra high performance liquid chromatography method development

Baksam, Vijayakumar; Saritha, Nimmakayala; S, Mohan; Shandilya, Sanjeev; Kumar, Pramod

doi:10.1002/jssc.202100050

Cited by 9 publications

(6 citation statements)

References 16 publications

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“…According to ICH, the method validations were performed for the parameter's specificity, linearity, detection limit, quantitation limit, accuracy, precision, and robustness, which were developed and optimized for the quantitative estimation of p-chlorophenol and unknown impurities of chlorzoxazone by RP-HPLC-UV method and genotoxic impurity 2-amino-4-chlorophenol by RP-HPLC-MS/MS method [35][36][37][38][39][40][41].…”

Section: Methods Validation Studymentioning

confidence: 99%

Stability‐indicating method for quantification of potential genotoxic impurity and other organic impurities of chlorzoxazone using hyphenated techniques

Nagulancha,

Rao

2023

Separation Science Plus

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A simple, reliable, and stability‐indicating RP‐HPLC‐UV method was developed and validated for the estimation of related substances (p‐chlorophenol and unknown impurities) of chlorzoxazone (skeletal muscle relaxant). Along with this as the compound contains a potential genotoxic impurity (2‐amino‐4‐chlorophenol), which needs to have more sensitivity in quantification, we have also developed and validated a separate RP‐HPLC‐mass spectrometry (MS)/MS method for the estimation of 2‐amino‐4‐chlorophenol impurity. Both methods (RP‐HPLC‐UV & RP‐HPLC–MS/MS) were validated in accordance with International Council for Harmonization Q2(R1) and were found to be precise, accurate, robust, linear, and specific with limit of quantification values established with respect to 100% of test concentration, 0.018% w/w of p‐chlorophenol by RP‐HPLC‐UV, and 2 ppm of 2‐amino‐4‐chlorophenol by RP‐HPLC–MS.

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Section: Methods Validation Studymentioning

confidence: 99%

Stability‐indicating method for quantification of potential genotoxic impurity and other organic impurities of chlorzoxazone using hyphenated techniques

Nagulancha,

Rao

2023

Separation Science Plus

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“…The importance of stressed/forced degradation is also stated in International Council for Harmonization (ICH) guidelines Q1A, Q1B, and Q2B. Profuse literature survey enlightens similar studies are carried out on various APIs using advanced hyphenated analytical techniques [6][7][8][9][10]. Apixaban is an oral medication.…”

Section: Introductionmentioning

confidence: 99%

Identification, isolation, and structural characterization of novel forced degradation products of apixaban using advanced analytical techniques

Salakolusu

Sharma

Katari

et al. 2022

J of Separation Science

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The current research explains the stress degradation behavior of Apixaban, which is an anticoagulant or blood thinner. The degradation was conducted using hydrolytic, oxidative, thermal, and photolytic conditions. Apixaban is relatively stable in oxidative, thermal, and photolytic conditions; however, considerable degradation was observed in acid and base hydrolysis. Degradation products were identified using ultra-high performance liquid chromatographymass spectrometry, isolated using semi-preparative high-performance liquid chromatography, and structural characterization by high-resolution mass spectrometry and nuclear magnetic resonance spectroscopy. A total of five degradation products were identified and isolated in acid and base degradation. Degradation products 1, 2, and 3 were observed in acid conditions, whereas in base conditions, along with those three, two more degradation products 4 and 5 were identified. The representative thing was that among the five degradation products, two sets of positional isomers 1, 4, and 2, 5 were observed; out of which 2 and 5 are novel. The remaining degradation products 1, 3, and 4 are already reported tentatively using a single analytical technique of mass analysis without any evidence from nuclear magnetic resonance spectroscopy. Hence, the present study focused on using high-resolution mass, and nuclear magnetic resonance spectroscopy data for concrete confirmation of structures for degradation products.

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“…United States Pharmacopeia (USP) and European Pharmacopeia both incorporated specification limits to set quantitative acceptable criteria for impurities/DPs. Thus, impurity profiling has become the most concerning task in the pharmaceutical industry to manufacture drugs of high quality [2][3][4][5][6].…”

Section: Introductionmentioning

confidence: 99%

Isolation, structure elucidation, and high‐performance liquid chromatography quantification of photolytic degradation impurities in acrivastine

Zeng

et al. 2022

J of Separation Science

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Acrivastine is a second-generation H1-receptor antagonist, and its structure is sensitive to ultraviolet. Four unknown and one reported degradation products can be detected in the ultraviolet radiation solutions of acrivastine. To improve the quality control of acrivastine, the photodegradation impurities were isolated and structurally elucidated. There are four new impurities (1-3 and 5), and one reported compound (4). The isolation strategy was designed as preparative high-performance liquid chromatography using a reversed phase column with volatile acid addition in the mobile phase, combined with preparative thinlayer chromatography using silica gel with alkaline addition in the mobile phase. Using the developed methods, five impurities (1-5) were efficiently purified after two or three chromatography runs with purities > 95%. The structures of compounds 1-5 are elucidated based on spectroscopy analysis of MS, and nuclear magnetic resonance spectroscopy. Using the impurity standard, the highperformance liquid chromatography method was developed and validated. The method was proved to be sensitive, accurate (Recovery% 96.1-107.7%), linear (0.15-0.75 μg/mL, R 2 > 0.996), robust, and specific, and it was successfully used to determine the degradation impurities of acrivastine and its formulation.

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Identification and characterization of Prothionamide degradation impurities by mass spectrometry, NMR spectroscopy, and ultra high performance liquid chromatography method development

Cited by 9 publications

References 16 publications

Stability‐indicating method for quantification of potential genotoxic impurity and other organic impurities of chlorzoxazone using hyphenated techniques

Stability‐indicating method for quantification of potential genotoxic impurity and other organic impurities of chlorzoxazone using hyphenated techniques

Identification, isolation, and structural characterization of novel forced degradation products of apixaban using advanced analytical techniques

Isolation, structure elucidation, and high‐performance liquid chromatography quantification of photolytic degradation impurities in acrivastine

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