Stability‐indicating HPLC method for simultaneous quantification of 14 impurities in excedrin tablet formulations and identification of new impurity by LC–MS in accelerated stability studies

Abstract

We developed novel stability-indicating HPLC method for simultaneous estimation of 14 impurities in excedrin tablet, a formulation with a combination of acetaminophen, aspirin, and caffeine. In addition, a new impurity that was generated through degradation of aspirin at high temperatures during the accelerated stability conditions was positively identified and confirmed, using liquid chromatography-mass spectrometry technique. The HPLC method was optimized using the Inertsustain C 18 , 250 × 4.6 mm, 5.0 μm column, employing simple gradient method. Forced degradation studies were performed under acidic, basic, oxidative and thermal conditions to prove the scope and stability-indicating the nature of the method. The optimized method was validated as per the International Conference on Harmonization guidelines. The HPLC method showed linearity from LOQ concentration to 21 μg mL −1 . Precision and intermediate precision values were <5% RSD. The validated HPLC method is currently applied for the routine testing of excedrin tablet formulations in quality control laboratories.

A novel RP‐HPLC refractive index detector method development and validation for determination of trace‐level alcohols (un‐sulfated) in sodium lauryl sulfate raw material

“…The proposed method was validated as per International Conference on Harmonization guidelines and US Pharmacopeia (USP) Compendia (Horacio et al, 2018; ICH, 2005; Dongala, Katakam, et al, 2019; Dongala, Katari, et al, 2019a, 2019b; Ashok, Thirupathi, Ravindra Kumar, & Jayashree, 2017; Murthy, Srinivas, Kumar, & Mukkanti, 2011; Subramanian, Katari, Dongala, & Jonnalagadda, 2020; Palakurthi, Dongala, Yalavarthi, & Anireddy, 2019; Kumar et al, 2013a, 2013b; Dongala, Katakam, et al, 2019; Dongala & Palakurthi, 2019; Dongala, Palakurthi, et al, 2019) based on the industry standard equipment.…”

Split-Half Tablets: A Complete Review for Analytical Testing

“…According to US FDA requirements (Guidance for industry, analytical procedures, and methods validation, FDA, 2000), a SIM [23][24][25][26][27][28][29][30][31][32] is described as a validated analytical procedure that quantifies the drug, free from process impurities, excipients, and degradation products precisely and accurately. The US-FDA supports that all assay methods for stability should be stability-indicating.…”

A simple high‐performance liquid chromatography method development for Carbidopa and Levodopa impurities: Evaluation of risk assessment before method validation by Quality by Design approach

“…In the current study, we have proposed an improved and alternative quality by design-based RP-HPLC method for the simultaneous determination of carbidopa, levodopa, and their impurities with a combination of entacapone in solid oral dosage forms. The purpose of the stabilityindicating analytical method is to provide evidence on how the quality of a drug substance or drug product varies with time under the influence of various environmental factors such as temperature, humidity, and light, and to establish a retest period for the drug substance or shelf life for the drug product and recommended storage condition [17][18][19][20]. Dongala et al [21] have demonstrated the importance of stability-indicating in the pharmaceutical industry.…”