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

Abstract

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.

An effective and stability‐indicating method development and optimization utilizing the Box–Behnken design for the simultaneous determination of acetaminophen, caffeine, and aspirin in tablet formulation

“…The current study aims to provide a direct QbD approach to HPLC procedure optimization for the determination of ACE, ASP, and CAF. To demonstrate the methodology's specificity, force degradation experiments were performed under various stress conditions for stability assessment (Ettaboina, Nakkala, et al, 2022; Katakam, Ettaboina, & Dongala, 2021; Mohan et al, 2020; Naresh & Madhuri, 2014; Yenda et al, 2021). The current study has significant advantages, which combine QbD evaluation with the chosen Critical Quality Attributes (CQA) and established rugged method conditions, and life‐cycle management approaches.…”

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

“…The present research study explains the analytical method development and validation for the OND pharmaceutical dosage form by identifying and controlling the impurities in the injectable formulation in a single method. A quality by design-based design of experiments (DoE) helps understand the significance of critical process parameters [25][26][27][28][29]. A multivariate DoE is utilized to evaluate operable and robust method conditions.…”

Stability‐indicating HPLC method development and validation of rivaroxaban impurities and identification of forced degradation products using LC–MS/MS

“…Rivaroxaban is used as an antithrombotic agent and exhibits potent anticoagulant effects (Perzborn et al, 2005; Roehrig et al, 2005). In the literature, a number of analytical methods have been described for the estimation of rivaroxaban and its impurities employing various techniques such as spectrophotometric methods (Celebier et al, 2014; Satyanarayana & Madhavi, 2012a; Sekaran et al, 2013), HPLC (Celebier et al, 2013; Dongala et al, 2021; Ettaboina et al, 2021, 2022; Jebaliya et al, 2015; Katakam, Dongala, & Ettaboina, 2021; Pinaz kasad, 2013; Pinaz kasad & Krishna, 2013; Prajapati & Patel, 2015; Rao et al, 2015; Rao & Sekar, 2013; Satyanarayana & Madhavi, 2012a, 2012b; Sekaran et al, 2013; Sekhar Chandra et al, 2012; Sunitha et al, 2014; Yenda et al, 2022), chiral HPLC (Ettaboina et al, 2021; Katakam et al, 2020; Katakam, Dongala, & Ettaboina, 2021; Prabhune et al, 2015), and LC–MS (Abdallah et al, 2015; Katakam, Dongala, & Ettaboina, 2021; Rao Nageswara & Krishna Rama, 2014). The main aim of this present research work is to develop a single method for the separation of enantiomers and its process‐related known and unknown impurities in drug substances containing rivaroxaban.…”