Determination and quantification of related substances and degradation products in bictegravir by full factorial design evaluated HPLC and mass spectrometry

R., Jythesh Kumar S.; Rao, Vandavasi Koteswara; Katari, Naresh Kumar; Narreddy, Siva jyothi; Kowtharapu, Leela Prasad

doi:10.1039/d2ay02106d

Cited by 6 publications

(2 citation statements)

References 32 publications

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“…In general, the technique should be enhanced or its robustness should be proven using the quality by design (QbD) approach, according to the present regulatory criteria, which are unambiguous. The robustness of the recently presented strategy was demonstrated using the QbD tool (Dandabattina et al, 2023; Jythesh Kumar et al, 2023; Konduru et al, 2022; Kowtharapu et al, 2022; Vemuri et al, 2022). The design of experiments based on QbD were carried out using Design‐Expert software version 13 (Stat‐Ease, Inc., Minneapolis, MN).…”

Section: Introductionmentioning

confidence: 99%

Quality by design tool–evaluated stability‐indicating ultra‐performance liquid chromatography method for the determination of drugs (ritonavir and darunavir) used to treat the human immunodeficiency virus/acquired immunodeficiency syndrome

Menda,

Kanuparthy,

Katari

et al. 2023

Biomedical Chromatography

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Ritonavir and darunavir were examined using a ultra‐performance liquid chromatography (UPLC) approach in pharmaceutical dosage forms. The small number of analytical studies that are currently available do not demonstrate the method's stability or nature. The study sought to assess both chemicals using a stability‐indicating approach with a relatively short run time. The HSS C18 (100 × 2.1 mm), 2‐mm column was used for the chromatographic separation, and isocratic elution was used to achieve this. In the mobile phase, methanol and 0.01 M phosphate buffer (pH 4.0) were included in a 60:40 (v/v) ratio. Throughout the analysis, the flow rate was kept at 0.2 mL min−1, and a photodiode array detector set to 266 nm was used to find the major components. The proposed method showed a linear response (r2 > 0.999), and the accuracy was between 98.0% and 102.0%. The precision data showed relative standard deviation ≤1.0%. The UPLC method for quantification of ritonavir and darunavir in pharmaceutical dosage forms using a very short run time of under a minute is the subject of the proposed article. To meet current regulatory criteria, the quality by design idea was used in the method performance verification.

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Section: Introductionmentioning

confidence: 99%

Quality by design tool–evaluated stability‐indicating ultra‐performance liquid chromatography method for the determination of drugs (ritonavir and darunavir) used to treat the human immunodeficiency virus/acquired immunodeficiency syndrome

Menda,

Kanuparthy,

Katari

et al. 2023

Biomedical Chromatography

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“…Considering the sensitivity and toxicity of this impurity (its consumption of high levels will cause cancer), we have selected the RP-HPLC-MS/MS technique for the estimation of 2-amino-4-chlorophenol in ppm level (Figure 1) [19][20][21][22][23]. Both methods were developed and validated considering the International Council for Harmonization (ICH) requirements, which met its acceptance criteria and were found to be specific, linear, accurate, precise, and robust [24][25][26][27][28]. The results of the forced degradation study confirmed that the developed RP-HPLC-UV method is stabilityindicating, in addition to being specific and selective in the separation and quantitative determination of organicrelated impurities of chlorzoxazone drug substance and drug product [29,30].…”

Section: Introductionmentioning

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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Stability‐indicating method development and validation for quantitative estimation of organic impurities of the antidiabetic drug glipizide in drug substance and pharmaceutical dosage form using HPLC

Nagulancha,

Vandavasi

2023

Biomedical Chromatography

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Glipizide is an antidiabetic drug used for the treatment of type 2 diabetes. A simple, reliable and robust reverse‐phase liquid chromatographic method (RP‐HPLC) was developed and validated as per International Conference on Harmonization Q2(R1) for estimating the impurities of glipizide in pharmaceutical formulations. The chromatographic separation was carried out on a Phenomenex Luna C18 (2), 250 × 4.6 mm, 5 μm with a binary solvent delivery system [MP‐A, a homogenous mixture of water and acetonitrile in a ratio of 90:10 (v/v) and 1 ml of orthophosphoric acid; and MP‐B, a homogenous mixture of water and acetonitrile in a ratio of 10:90 (v/v) and 1 ml of orthophosphoric acid] with a detection wavelength of 225 nm, a column temperature of 30°C, a flow rate of 1.5 ml/min, and an injection volume of 20 μl. All process, degradant and unknown impurities were separated well with a resolution >2.2 and were estimated accurately without any interference. The recovered values and regression values were 98.7–100.5% and R2 > 0.9999, respectively. The recovery and linearity studies covered the quantitation limit to 150% of the specification limit. The stability‐indicating properties of the developed RP‐HPLC method was assessed from the forced degradation studies. The developed method was successfully applied for real‐time sample analysis of the glipizide dosage form.

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Determination and quantification of related substances and degradation products in bictegravir by full factorial design evaluated HPLC and mass spectrometry

Abstract: Determining and quantifying novel Impurities and degraded impurities of a drug product is always a continuous challenge to enhancing the drug quality for patients' safety. Herein, our work deals with...

Cited by 6 publications

References 32 publications

Quality by design tool–evaluated stability‐indicating ultra‐performance liquid chromatography method for the determination of drugs (ritonavir and darunavir) used to treat the human immunodeficiency virus/acquired immunodeficiency syndrome

Quality by design tool–evaluated stability‐indicating ultra‐performance liquid chromatography method for the determination of drugs (ritonavir and darunavir) used to treat the human immunodeficiency virus/acquired immunodeficiency syndrome

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

Stability‐indicating method development and validation for quantitative estimation of organic impurities of the antidiabetic drug glipizide in drug substance and pharmaceutical dosage form using HPLC

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