METHOD DEVELOPMENT, VALIDATION AND FORCED DEGRADATION STUDIES OF RITONAVIR, AN ANTI-RETROVIRAL DRUG USING REVERSE PHASE-HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

Objective: A stability indicating reverse-phase high-performance liquid chromatography (RP-HPLC) method was developed and validated for the estimation of emtricitabine (EMT), rilpivirine (RIL), and tenofovir alafenamide (TAF) in combined dosage forms and its API.Methods: Chromatographic separation was achieved on Waters ACQUITY RP-HPLC with PDA detector having Zodiac C18 Column (250×4.6×5μ) using mobile phase mixture of phosphate buffer: acetonitrile in the ratio of 40:60 v/v at 262 nm.Results: The assay was performed with tablets, and the % assay was found to be 100.104 for EMT, 99.74 for RIL, and 102.41 for TAF which shows that the method is useful for routine analysis. The linearity was found to be linear with a correlation coefficient of 0.999, which shows that the method is capable of producing good sensitivity. The retention time (RT) of EMT, RIL, and TAF using optimum conditions was found to be 2.517, 3.273, and 6.697 min. Forced degradation studies (FDS) were performed on sample using acid, base, thermal, photolytic, and peroxide degradation.Conclusion: Due to its simplicity, rapidness, high precision, and low RT value, this method was successfully applied to the estimation of EMT, RIL, and TAF combined dosage form. The drugs were found to be stable at FDS, and the net degradation was found to be within the limits.

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REVERSE-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD DEVELOPMENT AND VALIDATION FOR SIMULTANEOUS ESTIMATION AND FORCED DEGRADATION STUDIES OF EMTRICITABINE, RILPIVIRINE, AND TENOFOVIR ALAFENAMIDE IN SOLID DOSAGE FORM

Asian Journal of Pharmaceutical and Clinical Research ◽

10.22159/ajpcr.2018.v12i1.28765 ◽

2019 ◽

Vol 12 (1) ◽

pp. 112

Author(s):

Juluri Krishna Dutta Tejaswi ◽

Govinda Rajan R

Keyword(s):

High Performance Liquid Chromatography ◽

Liquid Chromatography ◽

High Performance ◽

Dosage Form ◽

Forced Degradation ◽

Reverse Phase ◽

Rp Hplc ◽

Forced Degradation Studies ◽

Degradation Studies ◽

Tenofovir Alafenamide

Objective: A stability indicating reverse-phase high-performance liquid chromatography (RP-HPLC) method was developed and validated for the estimation of emtricitabine (EMT), rilpivirine (RIL), and tenofovir alafenamide (TAF) in combined dosage forms and its API.Methods: Chromatographic separation was achieved on Waters ACQUITY RP-HPLC with PDA detector having Zodiac C18 Column (250×4.6×5μ) using mobile phase mixture of phosphate buffer: acetonitrile in the ratio of 40:60 v/v at 262 nm.Results: The assay was performed with tablets, and the % assay was found to be 100.104 for EMT, 99.74 for RIL, and 102.41 for TAF which shows that the method is useful for routine analysis. The linearity was found to be linear with a correlation coefficient of 0.999, which shows that the method is capable of producing good sensitivity. The retention time (RT) of EMT, RIL, and TAF using optimum conditions was found to be 2.517, 3.273, and 6.697 min. Forced degradation studies (FDS) were performed on sample using acid, base, thermal, photolytic, and peroxide degradation.Conclusion: Due to its simplicity, rapidness, high precision, and low RT value, this method was successfully applied to the estimation of EMT, RIL, and TAF combined dosage form. The drugs were found to be stable at FDS, and the net degradation was found to be within the limits.

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Forced degradation studies on Naratriptan HCL by High Performance Liquid Chromatography.

10.3390/ecsoc-21-04808 ◽

2017 ◽

Author(s):

Vaibhav Kulkarni ◽

Kiran Sonawane

Keyword(s):

High Performance Liquid Chromatography ◽

Liquid Chromatography ◽

High Performance ◽

Forced Degradation ◽

Forced Degradation Studies ◽

Degradation Studies

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STABILITY-INDICATING REVERSE-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR THE SIMULTANEOUS QUANTIFICATION OF APIGENIN AND LUTEOLIN FROM ACHILLEA MILLEFOLIUM LINN

Asian Journal of Pharmaceutical and Clinical Research ◽

10.22159/ajpcr.2019.v12i4.31422 ◽

2019 ◽

pp. 169-172

Author(s):

GOMATHY SUBRAMANIAN ◽

S.N.MEYYANATHAN ◽

GOWRAMMA BYRAN

Keyword(s):

High Performance Liquid Chromatography ◽

Liquid Chromatography ◽

High Performance ◽

Degradation Products ◽

Forced Degradation ◽

Reverse Phase ◽

Chromatography Method ◽

Stability Indicating ◽

Degradation Studies ◽

Liquid Chromatography Method

Objective: A stability-indicating reverse-phase high-performance liquid chromatographic method was developed and validated for the analysis of apigenin and luteolin. The degradation behavior of apigenin and luteolin was investigated under different stress conditions as recommended by the International Conference on Harmonization (ICH). Methods: In the present study, a reversed-phase high-performance liquid chromatography method was developed and the resolution of the plant constituents was successfully achieved using Hibar Lichrospher C8 column with ultraviolet detector at a wavelength of 269 nm. The mobile phase consisted of methanol and 0.5% trifluoroacetic acid (80:20 v/v) at a flow rate of 1.0 ml/min. Both apigenin and luteolin were subjected to various stress degradation studies such as oxidation, acid and alkaline hydrolysis, and photolytic degradation. Results: The proposed method was found to be linear (1–5 μg/ml) with the linear correlation coefficient of R2=0.99. Although the degradation products of stressed conditions were not identified, the methods were able to detect the changes due to stress condition. Conclusion: The method provides good sensitivity and excellent precision and reproducibility. Forced degradation studies on apigenin and luteolin give information about their storage and intrinsic stability conditions considering the advanced pharmaceutical aspects of formulations.

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RP-HPLC assay method development for Paracetamol and Lornoxicam in combination and characterization of oxidative degradation products of Lornoxicam

Chemical Industry and Chemical Engineering Quarterly ◽

10.2298/ciceq120404084j ◽

2013 ◽

Vol 19 (4) ◽

pp. 471-484

Author(s):

Pritam Jain ◽

Miketa Patel ◽

Amar Chaudhari ◽

Sanjay Surana

Keyword(s):

Method Development ◽

Degradation Products ◽

Oxidative Degradation ◽

Assay Method ◽

Forced Degradation ◽

Control Analysis ◽

Reverse Phase ◽

Solution Form ◽

Forced Degradation Studies ◽

Degradation Studies

A simple, specific, accurate and precise reverse phase high pressure liquid chromatographic method has been developed for the simultaneous determination of Paracetamol and Lornoxicam from tablets and to characterize degradation products of Lornoxicam by reverse phase C18 column (Inertsil ODS 3V C-18, 250 x 4.6 mm, 5 ?). The sample was analyzed using Buffer (0.02504 Molar): Methanol in the ratio of 45:55, as a mobile phase at a flow rate of 1.5 mL/min and detection at 290 nm. The retention time for Paracetamol and Lornoxicam was found to be 2.45 and 9.40 min respectively. The method can be used for estimation of combination of these drugs in tablets. The method was validated as per ICH guidelines. The linearity of developed method was achieved in the range of 249.09 - 747.29 ?g/mL (r2=0.9999) for Paracetamol and 4.0125 - 12.0375 ?g/mL (r2=0.9999) for Lornoxicam. Recoveries from tablets were between 98 and 102%. The method was validated with respect to linearity, accuracy, precision, robustness and forced degradation studies which further proved the stability-indicating power. During the forced degradation studies lornoxicam was observed to be labile to alkaline hydrolytic stress and oxidative stress (in the solution form). However, it was stable to the acid hydrolytic, photolytic and thermal stress (in both solid and solution form). The degraded products formed were investigated by electrospray ionization (ESI) time-of-flight mass spectrometry, NMR and IR spectroscopy. A possible degradation pathway was outlined based on the results. The method was found to be sensitive with a detection limit of 0.193 ?g/ml, 2.768 ?g/ml and a quantitation limit of 0.638 ?g/ml, 9.137 ?g/ml for lornoxicam and paracetamol, respectively. Due to these attributes, the proposed method could be used for routine quality control analysis of these drugs in combined dosage forms.

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STABILITY INDICATING METHOD DEVELOPMENT AND VALIDATION OF FIMASARTAN BY REVERSE-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY IN BULK AND PHARMACEUTICAL DOSAGE FORM

Asian Journal of Pharmaceutical and Clinical Research ◽

10.22159/ajpcr.2021.v14i2.39919 ◽

2021 ◽

pp. 138-146

Author(s):

SRUTHI A ◽

UTTAM PRASAD PANIGRAHY

Keyword(s):

High Performance Liquid Chromatography ◽

Liquid Chromatography ◽

High Performance ◽

Dosage Form ◽

Method Development ◽

Internal Diameter ◽

Uv Detector ◽

Reverse Phase ◽

Pharmaceutical Dosage Form ◽

Rp Hplc

Objective: A rapid, sensitive and specific reverse phase High performance liquid Chromatography (RP-HPLC) method was developed for the estimation of Fimasartan in bulk and pharmaceutical dosage form. Method: The RP-HPLC analysis was performed isocratically on a Primacel C18 column (150 mm × 4.6 mm internal diameter, 5 μm particle size) using mobile phase of composition Acetonitrile and 0.1% orthophosphoric Acid in 80:20, v/v proportions with a flow rate of 0.8 ml/min. Results: The analyte was monitered with UV-detector at 265 nm. In the developed method Fimasartan elutes at a typical retention time of 2.4 min. The proposed method is having linearity in the concentration ranging from 5-30 μg/ml of Fimasartan. Conclusion: : The method was statistically validated and had been applied to analysis of the drug in bulk and pharmaceutical dosage form.

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