Development and Validation of a Stability-indicating Method for Ibrutinib: Identification and Separation of Degradation Products, Known and Genotoxic Impurities Using RP-HPLC/PDA and QDa Mass Detectors

Konduru, Naresh; Gundla, Rambabu; Katari, Naresh Kumar; Paidikondala, Kalyani; Reddy, A. Siva; Jagadabi, Varaprasad

doi:10.1080/22297928.2019.1673814

Cited by 22 publications

(17 citation statements)

References 8 publications

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“…IBR and the degraded product bands were well resolved. The reported stability indicating LC methods [5,6, 8‐10] uses gradient mobile phase system and less sensitive compared to developed HPTLC method. In LC method, separation efficiency varies with the column age while in HPTLC, every time new stationary phase plates (silica gel) are used which provides reproducible results in a short analysis time.…”

Section: Discussionmentioning

confidence: 99%

“…Literature survey of quantitative analysis of IBR revealed that various analytical methods have been reported for estimation of IBR. RP‐HPLC methods have been reported for the estimation of IBR in bulk and pharmaceutical dosage form [4–10]. Few UHPLC, UHPLC‐MS/MS, and UPLC‐MS/MS methods have been reported for the estimation of IBR in human plasma, human cerebrospinal fluid, and rat plasma respectively [11–13].…”

Section: Introductionmentioning

confidence: 99%

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Thin layer chromatographic method for separation and estimation of anticancer drug Ibrutinib in presence of its degradants

Shah

Patel

Mahajan

et al. 2021

Separation Science Plus

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A precise, accurate, and sensitive thin‐layer chromatographic method was developed for the estimation of anticancer drug Ibrutinib in synthetic mixture. The developed method uses precoated silica gel 60 F254 aluminum plates as stationary phase and Methanol: Ethyl acetate: Ammonia (2: 8: 0.2, v/v/v) as mobile phase. The densitometric analysis was carried out at the 286 nm under the reflectance mode and Rf was found to be 0.60 under optimized chromatographic condition. The linearity of the method was observed in the range of 100–500 ng/band. The developed method was validated as per the ICH guideline for the parameters like linearity, accuracy, precision, robustness, and specificity. As a part of specificity, a forced degradation study was carried out to know the possible amount of degradation under the various stress conditions such as acid, base hydrolysis, and oxidative stress degradation where the drug and the degradants band were well resolved from each other. The proposed method was successfully used for the estimation of IBR in a synthetic mixture.

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Section: Discussionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Thin layer chromatographic method for separation and estimation of anticancer drug Ibrutinib in presence of its degradants

Shah

Patel

Mahajan

et al. 2021

Separation Science Plus

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“…The method validation was performed per current ICH guidelines (Dongala et al, 2021;ICH, 2005;Konduru et al, 2020).…”

Section: Methods Validationmentioning

confidence: 99%

A simple isocratic LC method for quantification of trace‐level inorganic degradation impurities (ferricyanide, ferrocyanide, nitrite, and nitrate) in sodium nitroprusside injection and robustness by quality using design approach

Yenda

Katari

Dongala³

et al. 2021

Biomedical Chromatography

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This study developed and validated a trace-level quantification inorganic impurities method using reversed-phase HPLC and performed the robustness check using quality-by-design approach by varying the multiple factors simultaneously. This method is economical and simple and exhibits its stability-indicating nature [for the determination of ferrocyanide ([Fe(CN)] 4-), ferricyanide ([Fe(CN) and nitrite (NO 2 -)] in sodium nitroprusside (SNP) drug substance and liquid dosage form. Chromatographic separation was achieved using a USP L43 column (ACE PFP, 150 Â 4.6 mm, 3 μm) with a simple isocratic elution. The buffer consists of potassium dihydrogen phosphate (50 mM), tetrabutylammonium hydrogen sulfate (9 mM), and tetrabutylammonium hydroxide (25 mM). The buffer pH was adjusted to 7.2 with tetrabutylammonium hydroxide. The mobile phase was mixed with the buffer and acetonitrile (68:32 v/v). The flow rate was 0.8 mL/min, column temperature was maintained at 30 C, and injection volume was 5.0 μL. The SNP impurities were monitored at 225 nm using a UV detector. Further, the method was validated per the International Council for Harmonisation (ICH) guidelines, and forced degradation studies were carried out under different stress conditions. The detector responses were plotted against concentrations, and correlation was linear (r > 0.999) over the range of 0.8-7.5 μg/mL for ferricyanide; 1.0-37.5 μg/mL for SNP; and 0.2-7.5 μg/ mL for ferrocyanide, nitrite, and nitrate. The method repeatability was established for all the impurities with relative standard deviation (%), and the results were found to be less than 2.0.

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“…A stability-indicating method can quantify the response of the analyte and the presence of related substances in the degradation product. The stress study was performed on both drug products and placebo to investigate the interference of degradation products with related substances and analytes, need to analyze the acid, alkali, oxidative, thermal stress, and photo stress samples [35][36].…”

Section: Forced Degradation Studymentioning

confidence: 99%

Unique green chromatography method for the determination of serotonin receptor antagonist (Ondansetron hydrochloride) related substances in a liquid formulation, robustness by quality by design‐based design of experiments approach

Kowtharapu

Katari

Sandoval³

et al. 2022

J of Separation Science

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Serotonin receptor antagonist drug Ondansetron hydrochloride injectable formulation containing all related substances was identified and quantified by a single, simple, sensitive, eco-friendly, and green high-performance liquid chromatography method. The disseverment of all impurities was achieved with the Discovery Cyano (250 × 4.6) mm, 5 μm column. The gradient program was composed of pH 5.7 phosphate buffer as mobile phase A and acetonitrile as mobile phase B. The flow rate, column compartment temperature, and detection wavelengths were 0.9 mL/min, 30 • C, and 216 nm, respectively. The method was validated as per current regulatory guidelines. The obtained %relative standard deviation for the precision results was between 0.55 and 2.72% for all impurities. The correlation coefficient values from the linearity experiment for impurities and analyte were more than 0.995. The accuracy results were obtained between 88.4 and 113.0% for all impurities. Both sample and standard solutions showed 24 h stability at benchtop and refrigerator conditions. All impurities and analytes met the specificity and mass balance for all forced degradation conditions. Qualityby-design-based design of experiments was utilized to establish the method's robustness. Method greenness was assessed by using the current advanced tool green analytical procedure index, National Environmental Methods Index, and analytical eco-scale. K E Y W O R D Sanalytical eco-scale, design of experiments, green analytical procedure index, ondansetron hydrochloride, quality by design Article Related Abbreviations: ANOVA, analysis of variance; DoE, design of experiments; GAPI, Green Analytical Procedure Index; NEM, National Environmental Methods Index; OND, Ondansetron hydrochloride

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Development and Validation of a Stability-indicating Method for Ibrutinib: Identification and Separation of Degradation Products, Known and Genotoxic Impurities Using RP-HPLC/PDA and QDa Mass Detectors

Cited by 22 publications

References 8 publications

Thin layer chromatographic method for separation and estimation of anticancer drug Ibrutinib in presence of its degradants

Thin layer chromatographic method for separation and estimation of anticancer drug Ibrutinib in presence of its degradants

A simple isocratic LC method for quantification of trace‐level inorganic degradation impurities (ferricyanide, ferrocyanide, nitrite, and nitrate) in sodium nitroprusside injection and robustness by quality using design approach

Unique green chromatography method for the determination of serotonin receptor antagonist (Ondansetron hydrochloride) related substances in a liquid formulation, robustness by quality by design‐based design of experiments approach

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