scholarly journals Stability Indicating Method Development, Validation and Forced Degradation Study for Vilazodone Hydrochloride API

2021 ◽  
Vol 37 (1) ◽  
pp. 204-212
Author(s):  
Yogesh Jagdish Chaudhari ◽  
Rama Sadashiv Lokhande ◽  
Ravi Ramrathi Yadav
Keyword(s):  
Method Development ◽  
Oxidative Degradation ◽  
Hplc Method ◽  
Forced Degradation ◽  
Analytical Validation ◽  
Degradation Study ◽  
Related Substances ◽  
Stability Indicating Method ◽  
Basic Hydrolysis ◽  
Hplc Method Development

The current study describes the short, stability indicative HPLC method development and successive validation of Assay and Related Substances methods for Vilazodone Hydrochloride API. This study also covers Vilazodone process impurities viz. Impurity A and Impurity B. The chromatographic conditions for Related Substances and Assay are similar except sample concentration. The proposed method utilizes C18 column (15 cm X 4.6 mm, 5 µ, make ZORBAX SB) and mobile phase having Methanol and 0.05 M KH2PO4 (55: 45 v/v). The separation between all three analytes was achieved in less than five minutes. The analytical validation of these method was carried out successfully as per ICH and other international guidelines. The API was subject to various stress conditions like temperature, humidity, acidic and basic hydrolysis, oxidative degradation. The exposed samples analysed for impurities and assay. The mass balance for each condition was found more than 98%.

HPLC METHOD DEVELOPMENT, VALIDATION, AND FORCED DEGRADATION FOR SIMULTANEOUS ANALYSIS OF OXYCODONE AND NALTREXONEIN PHARMACEUTICAL DOSAGE FORM

INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (02) ◽  
pp. 31-38
Author(s):  
R. S. Ch Phani ◽  
◽  
K. R. S. Prasad ◽  
R. M Useni
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Hplc Method ◽  
Forced Degradation ◽  
Solution Stability ◽  
Pharmaceutical Dosage Form ◽  
Column Temperature ◽  
Degradation Study ◽  
Ich Guidelines ◽  
Hplc Method Development

A simple, precise and stability-indicating RP-HPLC method was developed for simultaneous quantification of oxycodone (OXCD) and naltrexone (NTRX) in combined dosage form. The developed method was validated with respect to precision, linearity, accuracy, robustness, ruggedness, sensitivity and solution stability. The method was developed with ammonium di hydrogen phosphate buffer (pH 5.0) and acetonitrile in a ratio of 55:45 (v/v) as mobile phase at a flow rate of 1.0 mL/minute over Intersil ODS C18 column (250 mm × 4.6 mm×5μ).The UV detection wavelength was fixed at 235 nm. The column temperature was maintained at ambient temperature. The method showed good linearity with correlation coefficient values of 0.9990 and 0.9994 for OXCD and NTRX. The percent recoveries of the two drugs found within the limits of 98.0–102.0%. The LOQ concentrations of OXCD and NTRX are 0.625 μg/ mL and 0.075 μg/mL, respectively. The LOD concentrations of OXCD and NTRX are 0.3125 μg/mL and 0.0375 μg/mL, respectively. According to ICH guidelines forced degradation study was validated.

Synthesis and Characterization of Potential and Degraded Impurities of Regadenoson

2020 ◽  
Vol 16 (8) ◽  
pp. 1130-1139
Author(s):  
Singaram Sathiyanarayanan ◽  
Chidambaram Subramanian Venkatesan ◽  
Senthamaraikannan Kabilan
Keyword(s):  
Mass Spectra ◽  
Degradation Products ◽  
Hplc Method ◽  
Forced Degradation ◽  
Spectroscopic Techniques ◽  
A2a Adenosine Receptor ◽  
Degradation Study ◽  
Related Substances ◽  
Adenosine Receptor Agonist

Background: Regadenoson is an A2A adenosine receptor agonist that is a coronary vasodilator and commonly used as a pharmacologic cardiac stressing agents. Methods: HPLC method was used for the analysis of related substances. The degraded impurities during the process were isolated and characterized by IR, Mass and NMR spectral analysis. Results: Forced degradation study of regadenoson under conditions of hydrolysis (neutral, acidic and alkaline) and oxidations suggested in the ICH Q1A(R2) was accomplished. The drug showed significant degradation under all the above conditions. On the whole, five novel degradation products were found under diverse conditions along with process related impurities which were not reported earlier. Conclusion: All the degradation products were well characterized by using advanced spectroscopic techniques like IR, 1H NMR, 13C NMR and Mass spectra. The identification of these impurities will be productive for the quality control during the production and stability behavior of the regadenoson drug substance.

scholarly journals Validation of Stability Indicating Method and Degradation Kinetic Study of Apremilast

2020 ◽  
Vol 10 (2) ◽  
pp. 76-85
Author(s):  
Jitesha Patel ◽  
Parin Chokshi ◽  
Rajashree Mashru
Keyword(s):  
Kinetic Study ◽  
Hplc Method ◽  
Forced Degradation ◽  
Order Kinetic ◽  
Degradation Kinetic ◽  
Degradation Study ◽  
Potassium Dihydrogen ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Rp Hplc

A novel stability indicating RP- HPLC method was developed for the estimation of Apremilast in bulk and marketed formulation. Separation was achieved by using Shimadzu HPLC Analytical Technologies Limited C18 (250 mm x 4.6 mm, 5µm) as stationary phase. The optimized mobile phase consist of potassium dihydrogen ortho phosphate (pH-3.2): acetonitrile in ratio of 40:60 %v/v with flow rate of 1mL/min by using methanol as diluent. Retention time of Apremilast was found to be 5.4 min which was estimated at wavelength 360nm. Linearity of Apremilast was observed in the concentration range of 50-400µg/mL with r² value of 0.9999. Assay of Apremilast tablet was found to be 99.14-100.75%. Stability indicating nature of RP- HPLC method was estimated by conducting degradation kinetic study. The forced degradation of Apremilast bulk indicate that degradation in acidic, alkali, oxidative and photolysis condition were found to be 21%, 6.5%, 25.7% and 3.9% respectively. The kinetic study of apremilast in alkali degradation followed first order kinetic study. The result indicate that the developed RP-HPLC method is suitable for estimation of Apremilast in presence of degradant product. The above method was validated as per ICH guideline. Keywords: Apremilast, RP-HPLC, Validation, Forced Degradation Study, Alkali Degradation Kinetic study

A new simple RP-HPLC Method development, Validation and Forced degradation studies of Bilastine

2021 ◽  
pp. 183-187
Author(s):  
Khushbu K. Patel ◽  
Arati M. Patel ◽  
C. N. Patel
Keyword(s):  
Retention Time ◽  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Forced Degradation ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Ich Guidelines ◽  
Hplc Method Development

A new simple, rapid, accurate and precise method for estimation of Bilastine in pharmaceutical dosage form by reverse phase liquid chromatography. The developed method employed mobile phase was Acetonitrile and Ammonium acetate pH 5.0 adjusted with glacial acetic acid with 85:15% v/v and flow rate 1.0ml/min. Method was developed using column C18 Water (150 × 4.6mm, 5µm) and detection wavelength was 215nm. The retention time was found to be 2.519 min. the proposed method was successfully applied to the determination of Bilastine in dosage form. High linearity of developed method was confirmed over concentration range of 25- 150 µg/ml and co-relation co-efficient is 0.996. The percentage RSD for precision and accuracy of the method was found to be less than 2%. The recovery was in the range of 99 – 102% and limit of detection was found to be 0.45µg/ml and limit of quantification was found to be 1.20µg/ml. Bilastine was found to degrade under acid and oxidation conditions. There was no interference of excipient and degradation product in retention time so method was specific. Analytical parameter such as precision, accuracy, limit of detection, limit of quantification and robustness were determined according to international Conference on Harmonization (ICH) guidelines.

scholarly journals Stability Indicating RP-HPLC Method Development for Related Substances of Anti-histamine Promethazine hydrochloride and its Validation study

2020 ◽  
Vol 36 (05) ◽  
pp. 889-896
Author(s):  
Nilesh Takale ◽  
Neelakandan Kaliyaperumal ◽  
Gopal Krishnan ◽  
Mannathusamy Mannathusamy ◽  
Raja Rajan Govindasamy
Keyword(s):  
Mobile Phase ◽  
Method Development ◽  
Potassium Hydroxide Solution ◽  
Hplc Method ◽  
Concentration Limit ◽  
Forced Degradation ◽  
Control Analysis ◽  
Related Substances ◽  
Rp Hplc ◽  
Promethazine Hydrochloride

A smooth, specific, precise, and accurate high-performance reverse phase (RP-HPLC) method for determining related substances in antihistamine Promethazine Hydrochloride (PMZ∙HCI) has been recorded. The RP-HPLC system is developed and tested in compliance with recommendations Q2(R1) of the International Council for Harmonization (ICH). Column 5m and reverse step with linear gradient elution is accomplished in Symmetry Shield RP8 (4.6 mm x 150 mm). Mobile phase A is 3.4% in the 7.0 pH water, modified to dilute potassium hydroxide solution. In contrast, the 60:40 mixture of acetonitrile and methanol combination as mobile phase B. The handled phase with a continuous flow rate of 1.0 ml min-1 is provided by choosing the wavelength 254 nm using a PDA/UV detector. The temperature of the column oven and sampler is 25°C and 4°C, respectively. The injection amount chosen is 10.0 μL. The method is linear in the quantitation limit range (LOQ) to 150 percent concerning the specification impurity concentration limit. Both impurities and PMZ have a correlation coefficient of greater than 0.999. The LOQ for all known impurities and PMZs has a specification limit of between 10 to 30%. The relative response factor for all four known impurities is calculated. The unexplained peaks are very different; the effects obtained are similar to the original values. There are no significant changes improvements to the suitability parameters, such as tailing factor, Plates theoretical sheets, and % RSD in Robustness Studies. The forced degradation analysis of PMZ∙HCI was performed. This RP-HPLC is descriptive, accurate and precise. This further defines the parameters of linearity, consistency and robustness used for regular quality control analysis.

scholarly journals METHOD DEVELOPMENT AND VALIDATION FOR SIMULTANEOUS QUANTIFICATION OF NETUPITANT AND PALONOSETRON IN BULK AND PHARMACEUTICAL DOSAGE FORM AND THEIR FORCED DEGRADATION STUDY BY RP-HPLC

2019 ◽  
pp. 119-123
Author(s):  
MANORANJANI M
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Forced Degradation ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Degradation Study ◽  
Simultaneous Quantification ◽  
Relative Standard

Objective: The present paper describes a simple, accurate, and precise reversed-phase high-performance liquid chromatography (HPLC) method for rapid and simultaneous quantification of netupitant (NTP) and palonosetron (PLS) in bulk and pharmaceutical dosage form. Methods: The chromatographic separation was achieved on Luna C18 (250 mm × 4.6 mm, 5 μ). Mobile phase contained a mixture of 0.1% orthophosphoric acid and acetonitrile in the ratio of 60:40 v/v, flow rate 1.0 ml/min, and ultraviolet detection at 222 nm. Results: The proposed method shows a good linearity in the concentration range of 60–900 μg/ml for NTP and 0.1–1.5 μg/ml for PLS under optimized conditions. All the precision and recovery results are in between 98 and 102%. In the entire robustness conditions, percentage of relative standard deviation is <2.0%. Degradation has minimum effect in stress condition and solutions are stable up to 24 h. This method is validated different parameters such as precision, linearity, accuracy, limit of detection, limit of quantification, ruggedness, robustness, and forced degradation study were determined according to the International Conference of Harmonization (ICH) Q2B guidelines. Conclusion: All the parameters of validation were found to be within the acceptance range of ICH guidelines. Since there is no HPLC method reported in the literature for the estimation of NTP and PLS in pharmaceutical dosage forms, there is a need to develop quantitative methods under different conditions to achieve improvement in sensitivity, selectivity, etc. Hence, the author has attempted to develop a validation and forced degradation for simultaneous quantification of NTP and PLS.

Stability Indicating RP-HPLC Method Development and Validation for Estimation of Diroximel Fumarate in bulk and its dosage forms

2021 ◽  
pp. 2603-2607
Author(s):  
Ramachandrapuram Kiranjyothi ◽  
Mahalingam Balakrishnan ◽  
Kothapalli Bannoth Chandrasekhar
Keyword(s):  
Method Development ◽  
Research Work ◽  
Dosage Forms ◽  
Hplc Method ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Rp Hplc ◽  
Validation Parameters ◽  
Hplc Method Development

Aim and objective: The aim of present research work is to develop validated RP-HPLC stability indicating method for the quantification of Diroximel Fumarate in bulk and its pharmaceutical dosage forms. Materials and methods: Chromatographic method was carried on C18 column (Waters 250mm x 4.6mm, 5m). Mobile phase was prepared by mixing water: Acetonitrile: 85% OPA: in the ratio of 70:30. The flow rate was 0.1 mL/min and the injection volume was 20μL. The absorbance maxima of Diroximel Fumarate was measured at 215nm. The retention time was found to be 2.390 min. Result: The method was proved to be specific and linear in the range of 50-150μg/mL with correlation coefficient of 0.999. The % RSD for precision was found to be less than 2% and the mean percentage recovery was 100.15%. All the validation parameters were statistically validated according to ICH guidelines and were found to be within acceptance criteria. Conclusion: The developed method was simple, specific, precise, accurate and robust. The described HPLC method can be successfully employed for the analysis of Diroximel Fumarate.

scholarly journals A novel RP- HPLC method development and forced degradation studies for semaglutide in active pharmaceutical ingredients and pharmaceutical dosage form

2019 ◽  
Vol 10 (2) ◽  
pp. 865-873
Author(s):  
Arun Kumar Kuna ◽  
Ganapathi S ◽  
Radha GV
Keyword(s):  
Method Development ◽  
Active Pharmaceutical Ingredient ◽  
Hplc Method ◽  
Forced Degradation ◽  
Simple Method ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Ingredients ◽  
Rp Hplc ◽  
Forced Degradation Studies ◽  
Hplc Method Development

This research objective is for the development of a specific and simple method to trace Semaglutide presence in active pharmaceutical ingredient and pharmaceutical dosages. As part of a study on Semaglutide drug, solvents of HPLC grade waters HPLC instrument (Empower software) with PDA detector, ultrasonicator (Make: Labman) and pH meter (Make: Adwa) are used. The Method was optimized with mobile phase with a composition of buffer and solvent were of 60:40%v/v, flow maintained was 1.0ml/min, the injection volume of 10µl, run time was 5min. All separations were performed with PDA detector and column used was Discovery C18 150 x 4.6mm, 5m. Results for the developed method are accurate and specific. The detection wavelength was 292 nm, the retention time for Semaglutide was 2.689min, linearity resulted with r2= 0.9998, % RSD for precision was 1.0; %mean recovery for accuracy was in the range of 99.73 to 100.29.  This study report is for industrial application for determining Semaglutide presence in pharmaceutical ingredient and dosages.

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