Stability‐indicating liquid chromatography method development and validation for impurity profiling of montelukast sodium in bulk drug and tablet dosage form

Baloxavir marboxil (BXM) is a polymerase acidic endonuclease inhibitor used as an antiviral drug. A simple, reliable, and robust liquid chromatographic method was developed and validated per International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH) Q2(R1) for estimating the assay and impurities of BXM in drug substance and pharmaceutical formulations. The chromatographic separation was carried out on C18 (100 × 4.6 mm, 5 μm) with binary solvent delivery system (A:0.1% trifluoroacetic acid in water; B:0.1% trifluoroacetic‐acid in acetonitrile) along with detection wavelength of 260 nm, column temperature of 57°C, flow of 1.2 mL/min and injection volume of 10 μL. All five known impurities and unknown impurities were separated well with resolution >1.7 and were estimated accurately without any interference. Recovered values and regression value were 99.5%–101.2% and R2 > 0.999, respectively. The recovery and linearity studies covered from 50% to 150% for assay, and quantitation limit, 120% for five BXM impurities. Stability‐indicating property of the HPLC developed method was assessed from the forced degradation studies. The mass spectral data of unknown impurity formed under oxidation stress condition were discussed. The developed method was also successfully utilized for stability sample analysis of drug substance and tablet dosage form.

Section: Introductionmentioning

confidence: 99%

Stability‐indicating method development and validation for quantitative estimation of assay and organic impurities of antiviral drug baloxavir marboxil in drug substance and pharmaceutical dosage form using HPLC and LC–MS methods

Nagulancha

Lakka

Rao

2023

“…for the separation and quantitative estimation of S ‐enantiomer of LA from both the drug substance and drug product (tablet dosage form). The stability‐indicating properties of the developed test method were assessed using forced degradation studies (Bakshi & Singh, 2002; Blessy et al, 2014; Boppy et al, 2022; Carr & Wahlich, 1990; Ettaboina, Katakam, & Dongala, 2022; Ettaboina, Nakkala, & Chathalingath, 2022; ICH, 1996; ICH, 2003; Katakam, Ettaboina, & Dongala, 2021; Katakam, Ettaboina, & Marisetti, 2021; Lakka & Goswami, 2012; Lakka et al, 2021, 2022; Lakkireddy et al, 2015; Mohan et al, 2022; Nagulancha et al, 2023; Narasimha et al, 2011, 2019, 2020, 2022; Siva et al, 2022; Snyder et al, 2010). The developed test method was validated in accordance with ICH (International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use) guidelines for specificity, linearity, accuracy, precision, and robustness (ICH, 2005; Narasimha & Chandrasekar, 2019).…”

Section: Introductionmentioning

confidence: 99%

“…for the separation and quantitative estimation of S-enantiomer of LA from both the drug substance and drug product (tablet dosage form). The stability-indicating properties of the developed test method were assessed using forced degradation studies (Bakshi & Singh, 2002;Blessy et al, 2014;Boppy et al, 2022;Carr & Wahlich, 1990;Ettaboina, Katakam, & Dongala, 2022;Ettaboina, Nakkala, & Chathalingath, 2022;ICH, 2003;Katakam, Ettaboina, & Dongala, 2021;Katakam, Ettaboina, & Marisetti, 2021;Lakka & Goswami, 2012;Lakka et al, 2021Lakka et al, , 2022Lakkireddy et al, 2015;Mohan et al, 2022;Nagulancha et al, 2023;Narasimha et al, 2011Narasimha et al, , 2020Narasimha et al, , 2022Siva et al, 2022;Snyder et al, 2010)…”

mentioning

confidence: 99%

Stability‐indicating normal‐phase HPLC method development for separation and quantitative estimation of S‐enantiomer of lacosamide in pharmaceutical drug substance and tablet dosage form

Vadagam

Haridasyam

Venkatanarayana

2023

Self Cite

Lacosamide (LA) is an antiepileptic medicine that is used to treat tonic–clonic seizures, partial‐onset seizures, mental problems, and pain. A simple, effective, and reliable normal‐phase liquid chromatographic technique was developed and validated to separate and estimate the enantiomer of (S‐enantiomer) LA in pharmaceutical drug substance and drug product. Normal‐phase LC was performed using USP L40 packing material (250 × 4.6 mm, 5 μm) and a mobile phase of n‐hexane and ethanol at 1.0 ml min−1. The detection wavelength, column temperature, and injection volume used were 210 nm, 25°C, and 20 μl, respectively. The enantiomers (LA and S‐enantiomer) were completely separated using a minimum resolution of 5.8 and accurately quantified without any interference in a 25‐min run time. Accuracy study for stereoselective and enantiomeric purity trials was conducted between 10 and 200%, with recovery values ranging from 99.4 to 103.1% and linear regression values >0.997. The stability‐indicating characteristics were assessed using forced degradation tests. The proposed normal‐phase HPLC technique is an alternate approach to the official monograph methods (USP and Ph.Eur.) of LA, and it was successfully used in the evaluation of release and stability samples for both tablet dosage forms and pharmaceutical substances.

“…Stability‐indicating liquid chromatography is a validated analytical test procedure that accurately and precisely measures the drug in drug substance or drug product free from impurities (process or degradation products), excipients used in drug formulation and solvent peaks used for the analysis. At present, high‐performance liquid chromatography (HPLC), ultra‐performance liquid chromatography (UPLC) and liquid chromatography coupled with mass spectrometry (LC–MS) are most frequently used to develop SIM and estimate the amount of impurities (Blessy et al, 2014; Lakka et al, 2021; Lakkireddy et al, 2015; Narasimha et al, 2019, 2020, 2022; Narasimha & Chandrasekar, 2019; Pasham et al, 2022). SIM plays an important role in analytical method development for the separation and quantitative estimation of organic impurities (process related impurities) and degradation products (DPs) which are most likely to be generated during the stress testing and storage of drugs owing to the environmental factors of heat, light and humidity.…”

Section: Introductionmentioning

confidence: 99%

“…At present, high-performance liquid chromatography (HPLC), ultraperformance liquid chromatography (UPLC) and liquid chromatography coupled with mass spectrometry (LC-MS) are most frequently used to develop SIM and estimate the amount of impurities (Blessy et al, 2014;Lakka et al, 2021;Lakkireddy et al, 2015;Narasimha et al, , 2020Narasimha et al, , 2022Pasham et al, 2022). SIM plays an important role in analytical method development for the separation and quantitative estimation of organic impurities (process related impurities) and degradation products (DPs) which are most likely to be generated during the stress testing and storage of drugs owing to the environmental factors of heat, light and humidity.…”

mentioning

confidence: 99%

Stability‐indicating liquid chromatography method development for assay and impurity profiling of amitriptyline hydrochloride in tablet dosage form and forced degradation study

Boppy

Haridasyam

Vadagam

et al. 2022

Self Cite

Amitriptyline hydrochloride is an antidepressant drug with sedative effects used to treat the symptoms of anxiety, agitation with depression and schizophrenia with depression. A reversed‐phase high‐performance liquid chromatography method was developed to separate and quantitatively determine the assay and four organic impurities of amitriptyline in tablet dosage form and bulk drugs using a C18 column in an isocratic elution mode with mobile phase consisting of a mixture of pH 7.5 phosphate buffer and methanol. The pH conditions used in the chromatographic separation are discussed. The stability‐indicating characteristics of the proposed method were proved using stress testing [5 m HCl at 80°C/1 h, 5 m NaOH at 80°C/1 h, H2O (v/w) at 80°C/1 h, 6% H2O2 (v/v) at 25°C/1 h, dry heat at 105°C/24 h and UV–vis light/4 days] and validated for specificity, detection limit, quantitation limit, linearity, precision, accuracy and robustness. For amitriptyline and its four known organic impurities, the quantitation limits, linearity and recoveries were in the ranges 0.25–3.0 μg/ml (r2 > 0.999) and 87.9–107.6%, respectively. The mass (m/z) spectral data of amitriptyline hydrochloride and its impurity are discussed. The proposed LC method is also suitable for impurity profiling and assay determination of amitriptyline in bulk drugs and pharmaceutical formulations.