scholarly journals Stability-Indicating HPLC Method for isoflavones aglycones analysis from Trifolium pratense L. extract

2020 ◽  
Vol 4 (1) ◽  
pp. 28-38
Author(s):  
Simony Martiny ◽  
Mairique Waszczuk ◽  
Samuel Kaiser ◽  
Marina Cardoso Nemitz ◽  
Valquiria Linck Bassani
Keyword(s):  
Hplc Analysis ◽  
Trifolium Pratense ◽  
Degradation Products ◽  
Hplc Method ◽  
Alkaline Media ◽  
Biochanin A ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
The Stability

The purpose of this study was to develop and validate a fast HPLC stability-indicating method for simultaneously quantifying the four main isoflavones in Trifolium pratense. Validation procedures followed the ICH requirements for complex matrices. The stability-indicating tests were performed by exposing the isoflavones to conditions of forced degradation and further analysis for verifying the formation of degradation products and their possible interferences in the HPLC analysis. The major isoflavones of Trifolium pratense proved to be stable against acid and oxidative media, thermodegradation, and photodegradation. However, they proved to be unstable in alkaline media, even for short periods of exposure like 2h. In this condition, in addition to the peaks corresponding to isoflavones, the HPLC analysis showed the presence of three additional peaks which were eluted at different retention times to the reference substances, without interfering in the quantification of the four analytes of interest, formononetin, biochanin A, daidzein and genistein. The method was validated following ICH guidelines showing to be specific, linear, precise, accurate, and robust.This first report concerning a stability-indicating method revealed that the proposed HPLC method reliably quantify the isoflavones and separate them from the degradation products in a short time of analysis.

scholarly journals Stability Study of Darunavir Ethanolate Tablets Applying a New Stability-Indicating HPLC Method

2013 ◽  
Vol 2013 ◽  
pp. 1-7 ◽  
Author(s):  
Josilene Chaves Ruela Corrêa ◽  
Cristina Helena dos Reis Serra ◽  
Hérida Regina Nunes Salgado
Keyword(s):  
Degradation Products ◽  
Hplc Method ◽  
Stability Study ◽  
Raw Material ◽  
Forced Degradation ◽  
The Novel ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
The Stability ◽  
Darunavir Ethanolate

Chemical and physical degradation of drugs may result in altered therapeutic efficacy and even toxic effects. Therefore, the aim of this work was to study the stability of darunavir and to develop and validate a liquid chromatography (LC) method to determine darunavir in raw material and tablets in the presence of degradation products. The novel method showed to be linear from 6.0 to 21.0 μg/mL, with high precision (CV < 2%) and accuracy (recuperation of 99.64%). It is simple and reliable, free of placebo interferences. The robustness of the method was evaluated by a factorial design using seven different parameters. Forced degradation study was done under alkaline, acidic, and oxidative stress at ambient temperature and by heating. The LC method was able to quantify and separate darunavir and its degradation products. Darunavir showed to be unstable under alkaline, acid, and oxidative conditions. The novelty of this study is understanding the factors that affect darunavir ethanolate stability in tablets, which is the first step to unravel the path to know the degradation products. The novel stability-indicating method can be used to monitor the drug and the main degradation products in low concentrations in which there is linearity.

DEVELOPMENT OF A VALIDATED STABILITY-INDICATING METHOD FOR ESTIMATION OF ETHIONAMIDE IN TABLETS BY RP-HPLC AND CHARACTERIZATION OF ITS ISOLATED ALKALI DEGRADATION PRODUCT

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (01) ◽  
pp. 20-27
Author(s):  
Sandeep S. Sonawane ◽  
◽  
Akshay S. Patil ◽  
Santosh S. Chhajed ◽  
Dimple S. Lalchandani ◽  
...  
Keyword(s):  
Degradation Product ◽  
Elevated Temperatures ◽  
Degradation Products ◽  
Hplc Method ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Rp Hplc ◽  
Photolytic Degradation ◽  
Alkali Hydrolysis

A simple, accurate, reproducible and specific stability-indicating RP-HPLC method was developed for estimation of ethionamide in tablets. Ethionamide was exposed to acid, alkali and neutral hydrolysis at elevated temperatures, to thermolytic degradation, peroxide-mediated oxidation at room temperature in dark and to photolytic degradation. The drug was found stable to thermolytic and photolytic conditions and to neutral hydrolysis. However, substantial degradation was obtained in acid and alkali hydrolysis and complete degradation in peroxide-medicated oxidation. Similar degradation behavior was observed when ethionamide tablets were exposed to the mentioned forced degradation conditions. The method showed adequate resolution of drug from its potential degradation products on C18 (250 × 4.6 mm, 5µ) column using mobile phase of methanol: water (50: 50 % V/V) at 1 mL/min. The drug and its potential degradation products were detected at 290 nm. The method was validated as per the ICH Q2(R1) guidelines. The enrichment of the alkali degradation product was performed and isolated by preparative TLC and further confirmed by NMR and IR spectroscopy.

Development and Validation of a Stability Indicating RP-HPLC Method for Hydrocortisone Acetate Active Ingredient, Propyl Parahydroxybenzoate and Methyl Parahydroxybenzoate Preservatives, Butylhydroxyanisole Antioxidant, and Their Degradation Products in a Rectal Gel Formulation

2015 ◽  
Vol 98 (1) ◽  
pp. 27-34 ◽  
Author(s):  
Magda Ascaso ◽  
Pilar Pérez-Lozano ◽  
Mireia García ◽  
Encarna García-Montoya ◽  
Montse Miñarro ◽  
...  
Keyword(s):  
Active Ingredient ◽  
Active Substance ◽  
Degradation Products ◽  
Gradient Elution ◽  
Hplc Method ◽  
Array Detector ◽  
Hydrocortisone Acetate ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
The Stability

Abstract A stability indicating method was established through a stress study, wherein different methods of degradation (oxidation, hydrolysis, photolysis, and temperature) were studied simultaneously to determine the active ingredient hydrocortisone acetate, preservatives propyl parahydroxybenzoate, and methyl parahydroxybenzoate, antioxidant butylhydroxyanisole (BHA), and their degradation products in a semisolid dosage gel form. The proposed method was suitably validated using a Zorbax SB-Phenyl column and gradient elution. The mobile phase consisted of a mixture of methanol, acetonitrile, and water in different proportions according to a planned program at a flow rate of 1.5 mL/min. The diode array detector was set at 240 nm for the active substance and two preservatives,and 290 nm for BHA. The validation study was conducted according to International Conference on Harmonization guidelines for specificity, linearity, repeatability, precision, and accuracy. The method was usedfor QC of hydrocortisone acetate gel and for the stability studies with the aim of quantifying the active substance, preservatives, antioxidant, and degradation products. It has proved to be suitable as a fast and reliable method for QC.

scholarly journals Development and validation of the stability-indicating LC-UV method for the determination of cefoselis sulphate

2012 ◽  
Vol 10 (1) ◽  
pp. 121-126 ◽  
Author(s):  
Przemysław Zalewski ◽  
Judyta Cielecka-Piontek ◽  
Anna Jelińska
Keyword(s):  
Mobile Phase ◽  
Degradation Products ◽  
Kinetic Studies ◽  
Hplc Method ◽  
Assay Method ◽  
Forced Degradation ◽  
Stability Indicating ◽  
The Stability ◽  
Development And Validation

AbstractThe stability-indicating LC assay method was developed and validated for quantitative determination of cefoselis sulphate in the presence of degradation products formed during the forced degradation studies. An isocratic, RP-HPLC method was developed with C-18 (250 × 4.6 mm, 5 µm) column and 12 mM ammonium acetate-acetonitrile (95:5 V/V) as a mobile phase. The flow rate of the mobile phase was 1.0 mL min−1. Detection wavelength was 260 nm and temperature was 30°C. Cefoselis similarly to other cephalosporins was subjected to stress conditions of degradation in aqueous solutions including hydrolysis, oxidation, photolysis and thermal degradation. The developed method was validated with regard to linearity, accuracy, precision, selectivity and robustness. The method was applied successfully for identification and determination of cefoselis sulphate in pharmaceuticals and during kinetic studies.

Development and Validation of a Stability-Indicating HPLC Method for the Analysis of Cabazitaxel in Jevtana® Concentrate-Solvent Leftover Samples

2020 ◽  
Vol 16 ◽  
Author(s):  
Hedvig Arnamo ◽  
Michel Hillebrand ◽  
Alwin Huitema ◽  
Bastiaan Nuijen ◽  
Hilde Rosing ◽  
...  
Keyword(s):  
Degradation Product ◽  
High Performance ◽  
Uv Light ◽  
Degradation Products ◽  
Physical Stability ◽  
Solvent Mixture ◽  
Hplc Method ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Stability Indicating Method

Aim/Background: In this study, a stability-indicating method of the anticancer agent cabazitaxel was developed and validated. This method will be used to determine the chemical stability of commercially available concentrate-solvent mixture cabazitaxel (Jevtana®) to examine the possibility of multi-dosing from the same product vial after storage. The impossibility to re-use leftovers today is contributing to an unnecessary and significant financial waste. Methods: A forced degradation study of cabazitaxel was performed under different conditions to produce degradation products. Acidic, basic, oxidation, heat, and ultraviolet (UV) light conditions were tested. The method to determine the stability was developed so that potential degradation products would be shown in the UV spectra after separation from cabazitaxel with a C18 column in a high-performance liquid chromatography (HPLC) system. The only degradation product occurring during storage in room temperature and ambient light was identified by accurate mass Orbitrap Mass Spectrometry. Results/Conclusion: A stability-indicating method for cabazitaxel (Jevtana ®) concentrate-solvent mixture has been developed. We demonstrated that this method can be applied to stability studies with the purpose of multi-dosing cabazitaxel from a chemical/physical stability perspective within the tested period of time and conditions. As an addition, the only naturally occurring degradation product found has been identified and a degradation reaction has been suggested.

scholarly journals Validated Stability Indicating RP-HPLC Method for Simultaneous Estimation of Codeine Phosphate and Chlorpheniramine Maleate from Their Combined Liquid Dosage Form

2013 ◽  
Vol 2013 ◽  
pp. 1-7 ◽  
Author(s):  
Ramakrishna Kommana ◽  
Praveen Basappa
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Codeine Phosphate ◽  
Chlorpheniramine Maleate ◽  
Combination Drug ◽  
Stability Indicating ◽  
Rp Hplc

The present paper describes the development of quick stability indicating RP-HPLC method for the simultaneous estimation of codeine phosphate and chlorpheniramine maleate in the presence of its degradation products, generated from forced degradation studies. The developed method separates codeine phosphate and chlorpheniramine maleate in impurities/degradation products. Codeine phosphate and chlorpheniramine maleate and their combination drug product were exposed to acid, base, oxidation, dry heat, and photolytic stress conditions, and the stressed samples were analysed by proposed method. The proposed HPLC method utilizes the Shimadzu HPLC system on a Phenomenex C18 column (, 5 μ) using a mixture of 1% o-phosphoric acid in water : acetonitrile : methanol (78 : 10 : 12) mobile phase with pH adjusted to 3.0 in an isocratic elution mode at a flow rate of 1 mL/min, at 23°C with a load of 20 μL. The detection was carried out at 254 nm. The retention time of codeine phosphate and chlorpheniramine maleate was found to be around 3.47 min and 9.45 min, respectively. The method has been validated with respect to linearity, robustness, precision, accuracy, limit of detection (LOD), and limit of quantification (LOQ). The developed validated stability indicating HPLC method was found to be simple, accurate, and reproducible for the determination of instability of these drugs in bulk and commercial products.

A New, Rapid and Simple RP-HPLC Method for Stability Quantification of a Protease Inhibitor in Tablets

2021 ◽  
Author(s):  
Rochele Cassanta Rossi ◽  
Josué Guilherme Lisbôa Moura ◽  
Vanessa Mossmann ◽  
Patrícia Weimer ◽  
Pedro Eduardo Fröehlich
Keyword(s):  
Quality Control ◽  
Protease Inhibitor ◽  
Degradation Products ◽  
Gradient Elution ◽  
Hplc Method ◽  
Array Detector ◽  
Forced Degradation ◽  
Control Analysis ◽  
Quality Control Laboratory ◽  
The Stability

Abstract Fosamprenavir calcium is a protease inhibitor widely used in the treatment and prevention of human immunodeficiency virus and acquired immunodeficiency syndrome. This protease inhibitor serves as a prodrug of amprenavir, offering better oral bioavailability. Although this drug was approved by the FDA in 2003, there are few methods established for quantifying the stability for quality control analysis of fosamprenavir-coated tablets. The purpose of the study was to develop and validate a method for determining the stability of fosamprenavir-coated tablets (Telzir®) that may be applied by any quality control laboratory. Chromatographic separation was performed using a Vertical RP-18 column programmed to run a gradient elution with sodium acetate buffer and acetonitrile. Flow rate was 1.2 mL min−1 for a total run time of 15 min. Ultraviolet detection was set at 264 nm and the use of a photodiode array detector in scan mode allowed selectivity confirmation by peak purity evaluation. The analyte peak was found to be adequately separated from degradation products generated during forced degradation studies. Thus, the proposed method was found to accurately indicate stability and was sufficient for routine quantitative analysis of fosamprenavir in coated tablets without interference from major degradation products and excipients.

scholarly journals Development of a Stability Indicating Method for Simultaneous Analysis of Five Water-Soluble Vitamins by Liquid Chromatography

2018 ◽  
Vol 3 (4) ◽  
pp. 207-218 ◽  
Author(s):  
Mouloud Yessaad ◽  
Lise Bernard ◽  
Daniel Bourdeaux ◽  
Philip Chennell ◽  
Valérie Sautou
Keyword(s):  
Liquid Chromatography ◽  
Degradation Products ◽  
Pharmaceutical Preparations ◽  
Water Soluble ◽  
Alkaline Solutions ◽  
Array Detector ◽  
Forced Degradation ◽  
Metaphosphoric Acid ◽  
Stability Indicating ◽  
Stability Indicating Method

Abstract Background Water-soluble vitamins are often included simultaneously in pharmaceutical formulations as food complements or in parenteral nutrition mixtures. Given their sensitivity to heat, light or pH variations, it is important to study their stability using validated stability indicating methods. We thus aimed to validate a liquid chromatography (LC) stability-indicating method for the simultaneous quantification of 5 water-soluble vitamins. Methods We analyzed four water-soluble B vitamins (nicotinamide, pyridoxine, folic acid, cyanocobalamin) and ascorbic acid using a LC method with diode array detector. They were separated on a C18 stationary phase under gradient elution of solvent A [0.2 % of metaphosphoric acid in water and acetonitrile 98:2] and solvent B (100 % acetonitrile). All vitamins were subjected to forced degradation conditions and we showed that the obtained degradation products didn’t interfere with the vitamins. Results The method allows the separation of the 5 water-soluble vitamins in a 30 minute run without any interference from the breakdown products obtained with acid/alkaline solutions, hydrogen peroxide, temperature and light. It meets all the qualitative and quantitative criteria for validation with an acceptable accuracy and good linearity. Conclusions This stability-indicating method can be used for carrying out stability studies of water-soluble vitamins in pharmaceutical preparations.

scholarly journals SIMULTANEOUS ESTIMATION, VALIDATION, AND FORCED DEGRADATION STUDIES OF BETAHISTINE DIHYDROCHLORIDE AND DOMPERIDONE IN A PHARMACEUTICAL DOSAGE FORM USING RP-HPLC METHOD

2018 ◽  
Vol 11 (10) ◽  
pp. 125
Author(s):  
Vaishali Mistry ◽  
Rohan Mishra
Keyword(s):  
Hplc Method ◽  
Base Hydrolysis ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Uv Detector ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Betahistine Dihydrochloride ◽  
The Stability

Objective: This study describes the stability-indicating reverse-phase high-performance liquid chromatography (RP-HPLC) method for simultaneous estimation of betahistine dihydrochloride and domperidone in pharmaceutical dosage forms.Methods: The proposed RP-HPLC method was developed using Shimadzu Prominence-i LC-2030 HPLC system equipped with UV detector and chromatographic operation was carried on Shim-pack C18 (250 mm×4.6 mm, 5 μ) column at a flow rate of 1 ml/min and the run time was 10 min. The mobile phase consisted of methanol and water in the ratio of 80:20% v/v and eluents were scanned using a UV detector at 244 nm.Results: The retention time of betahistine dihydrochloride and domperidone was found to be 2.3 and 3.6 min, respectively. A linearity response was observed in the concentration range of 9.6 μg/ml–22.4 μg/ml for betahistine dihydrochloride and 6–14 μg/ml for domperidone, respectively. Limit of detection and limit of quantification for betahistine dihydrochloride were 0.52 μg/ml and 1.58 μg/ml and for domperidone are 0.64 μg/ml and 1.94 μg/ml, respectively.Conclusion: The stability-indicating method was developed by subjecting drugs to stress conditions such as acid and base hydrolysis, oxidation, photo and thermal degradation, and degraded products formed were resolved successfully from samples.

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