Development of HPLC Method for Estimation of Darunavir Related Substance in Formulation

Rathod, Sumanth; Pounikar, Anita R; Umekar, Milind J.; Gupta, Kanishk

doi:10.26717/bjstr.2020.28.004624

BJSTR

2020

DOI: 10.26717/bjstr.2020.28.004624

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Development of HPLC Method for Estimation of Darunavir Related Substance in Formulation

Sumanth Rathod¹,

Anita R Pounikar²,

Milind J. Umekar³

et al.

Abstract: A simple, specific and validated reverse phase high performance liquid chromatography method was developed for determination of drug related substances (impurity) of Darunavir in formulation. Method development includes optimization of stationary phase (column) and mobile phase flow rate for the resolution of six known impurities and one unknown impurity and Darunavir. Development of HPLC method for estimation of Darunavir related substance in formulation was carried out on Zorbax SB-C8, 250 x 4.6mm, 5µm by us… Show more

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Cited by 2 publications

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Identification, Isolation, and Structural Characterization of Novel Forced Degradation Products of Darunavir Using Advanced Analytical Techniques Like UPLC–MS, Prep-HPLC, HRMS, NMR, and FT-IR Spectroscopy

Modini

Ranga

Puppala³

et al. 2022

Chromatographia

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Since the stability of the pharmaceuticals plays a crucial role in efficacy and safety while using them in the treatment of disorders, the evaluation of purity and impurity profiling of pharmaceuticals is of utmost importance using efficient analytical techniques. The present study explains the identification, isolation, and characterization of stress degradation products of the anti-human immunovirus drug Darunavir. The degradation study was performed to evaluate the stability profile of Darunavir in different stress conditions like hydrolytic, oxidative, thermal, and photolytic conditions as per the ICH guidelines. Degradation products were identified using ultra-performance liquid chromatography coupled with mass spectrometry, isolated using semi-preparative high-performance liquid chromatography, and structural characterization by HRMS and 1 H, 13 C NMR (1D, 2D). Darunavir is relatively stable in oxidative, thermal, and photolytic conditions; however, considerable degradation was observed in acid and base hydrolysis. A total of five degradation products were identified and isolated in acid and base degradation. DP-1, DP -2, & DP-3 were observed in acid conditions, whereas in base conditions, along with DP-2, two more DPs, i.e., DP-4 & DP-5, were identified. Among the five DPs, two degradation products, namely DP-1 : N-(4-(N-(3-amino-2-hydroxy-4-phenylbutyl)-N-isobutylsulfamoyl) phenyl) acetimidamide. & DP-3 : hexahydrofuro[2,3-b]furan-3-yl(4-((4-acetimidamido-N-isobutylphenyl)sulfonamido)-3-hydroxy-1-phenylbutan-2-yl)carbamate, are novel, remaining degradation products DP-2: 4-amino-N-(3-amino-2-hydroxy-4-phenylbutyl)-N-isobutylbenzenesulfonamide, DP-4 : 4-amino-N-(((5S)-4-benzyl-2-oxooxazolidin-5-yl) methyl) -N-isobutyl benzenesulfonamide and DP-5 : methyl ((3S)-4-((4-amino-N-isobutylphenyl) sulfonamido)-3-hydroxy-1-phenylbutan-2-yl) carbamate are already reported tentatively using a single analytical technique coupled with mass analysis without any evidence from NMR and IR data. Hence, the present study focused on using High-Resolution Mass, 1D, and 2D 1 H, 13 C NMR data for concrete confirmation of structures for degradation products. Supplementary Information The online version contains supplementary material available at 10.1007/s10337-022-04226-z.

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Identification, Isolation, and Structural Characterization of Novel Forced Degradation Products of Darunavir Using Advanced Analytical Techniques Like UPLC–MS, Prep-HPLC, HRMS, NMR, and FT-IR Spectroscopy

Modini

Ranga

Puppala³

et al. 2022

Chromatographia

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Development of a Validated Stability-Indicating HPLC Method for Vinpocetine in the Presence of Potential Impurities in Tablet Dosage Form by Multiresponse Optimization

Karaer

Dinç‐Zor

Aşçı

2021

Journal of AOAC INTERNATIONAL

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Background Vinpocetine has been prescribed for the treatment of ischemic brain diseases for many years. The drug, which has side effects such as headache, flushing, and decreased blood pressure, is not found in nature, but it can be synthesized by several approaches. Objectives A simple, rapid, selective, stability-indicating high performance liquid chromatographic method was developed for the simultaneous estimation of vinpocetine and their potential impurities in a tablet formulation. Methods Optimum HPLC conditions were tried to be determined by statistical experimental design method. The proposed method was validated as per the ICH guidelines. Stress study was used to demonstrate the stability-indicating ability of the developed method in the quantification of vinpocetine and potential impurities within the same run. Results According to multi-response optimization using the Derringer’s desirability function, the mobile phase consisted of acetonitrile: Phosphate Buffer (pH 6.0) in the ratio of 65:35 ʋ/ʋ at a flow rate of 1.7 mL/min. Significant degradations were observed for the drug product under acid hydrolysis and alkali hydrolysis. The new method showed reasonable detection and quantification limits with good selectivity, precision, linearity and recovery. Conclusions These validation results have shown that this method is suitable for quantitative determination of vinpocetine and its impurities in quality control laboratories. Highlights A reliable and rapid HPLC method which was optimized with response surface methodology and multi-response optimization based on Derringer’s desirability function was developed for the simultaneous analysis of vinpocetine and its impurities in a tablet formulation.

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Development of HPLC Method for Estimation of Darunavir Related Substance in Formulation

Cited by 2 publications

References 7 publications

Identification, Isolation, and Structural Characterization of Novel Forced Degradation Products of Darunavir Using Advanced Analytical Techniques Like UPLC–MS, Prep-HPLC, HRMS, NMR, and FT-IR Spectroscopy

Identification, Isolation, and Structural Characterization of Novel Forced Degradation Products of Darunavir Using Advanced Analytical Techniques Like UPLC–MS, Prep-HPLC, HRMS, NMR, and FT-IR Spectroscopy

Development of a Validated Stability-Indicating HPLC Method for Vinpocetine in the Presence of Potential Impurities in Tablet Dosage Form by Multiresponse Optimization

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