scholarly journals Application and Validation of Simple Isocratic HPLC-UV-DAD Method with Dual Wavelength Detection for Ivabradine Determination and Its Application in the Study of Stress Degradation

2017 ◽  
Vol 2017 ◽  
pp. 1-7 ◽  
Author(s):  
Joanna Nowakowska ◽  
Piotr Pikul ◽  
Marcin Marszałł ◽  
Krzesimir Ciura
Keyword(s):  
Degradation Products ◽  
Hplc Method ◽  
Simple Method ◽  
Degradation Study ◽  
Modern Drug ◽  
Stress Degradation ◽  
Isocratic Hplc ◽  
Cardiac Energy ◽  
Wavelength Detection

Ivabradine is a modern drug that selectively lowers the heart rate, improves cardiac energy balance, and reduces heart’s demands for oxygen and energy. Due to the chemical nature of ivabradine, which absorbs light at 207 nm and 286 nm, its detection was performed at two wavelengths. A Knauer C8 column was used to develop the RP-HPLC method for determination of ivabradine. The proposed method was linear from 5 to 100 µg/ml (r>0.999) for both wavelengths and limits of detection (LOD) and limits of quantification (LOQ) were 0.33 and 1.09 µg/ml for 207 nm and 1.19 and 3.97 µg/ml for 286 nm, respectively. After validation, the investigated method was applied to a stress degradation study. Numerous degradation products were formed from ivabradine solutions through alkaline and acid hydrolysis, oxidation, and photolysis. The largest numbers of degradation products were found in the sample exposed to 24 h radiation and alkaline hydrolysis (eight and six products, resp.). Finally, the simple method using HPLC-UV-DAD was developed and validated. Its usefulness for the monitoring of possible degradation products was demonstrated.

Development and validation of a fast and simple HPLC method for the simultaneous determination of aniline and its degradation products in wastewater

2016 ◽  
Vol 8 (30) ◽  
pp. 5949-5956 ◽  
Author(s):  
Soumia Boulahlib ◽  
Ali Boudina ◽  
Kahina Si-Ahmed ◽  
Yassine Bessekhouad ◽  
Mohamed Trari
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Reversed Phase ◽  
Hplc Method ◽  
Array Detector ◽  
Simple Method ◽  
Photodiode Array Detector ◽  
Photodiode Array ◽  
Development And Validation

In this study, a rapid and simple method based on reversed-phase high performance liquid chromatography (RP-HPLC) using a photodiode array detector (PDA) for the simultaneous analysis of five pollutants including aniline and its degradation products, para-aminophenol, meta-aminophenol, ortho-aminophenol and phenol, was developed.

scholarly journals DEVELOPMENT AND VALIDATION OF STABILITY INDICATING RP-HPLC METHOD FOR DETERMINATION OF β-ACETYLDIGOXIN

2016 ◽  
Vol 9 (1) ◽  
pp. 54
Author(s):  
Megha Sharma ◽  
Neeraj Mahindroo
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Hplc Method ◽  
Stability Study ◽  
Array Detector ◽  
Forced Degradation ◽  
Simple Method ◽  
Stability Indicating ◽  
Rp Hplc

Objective: The objective of the present study was to develop and validate a novel stability indicating reverse phase-high performance liquid chromatography (RP-HPLC) method for determination of β-acetyldigoxin, an active pharmaceutical ingredient (API).Methods: The chromatographic separation was carried out on Agilent Technologies 1200 series HPLC system equipped with photo diode array detector and C-18 (4.6x250 mm, 5 µ) column. The mobile phase consisted of water: acetonitrile (65:35 v/v), delivered at a flow rate of 1.5 ml/min and eluents were monitored at 225 nm.Results: The retention time of β-acetyldigoxin was 9.2 min. The method was found to be linear (R2= 0.9995) in the range of 31.25-500 µg/ml. The accuracy studies showed the mean percent recovery of 101.02%. LOD and LOQ were observed to be 0.289 µg/ml and 0.965 µg/ml, respectively. The method was found to be robust and system suitability testing was also performed. Forced degradation analysis was carried out under acidic, alkaline, oxidative and photolytic stress conditions. Significant degradation was observed under tested conditions, except for oxidative condition. The method was able to separate all the degradation products within runtime of 20 min and was able to determine β-acetyldigoxin unequivocally in presence of degradation products.Conclusion: The novel, economic, rapid and simple method for analysis of β-acetyldigoxin is reported. The developed method is suitable for routine quality control and its determination as API, and in pharmaceutical formulations and stability study samples.

A New Validated Stability Indicating RP-HPLC Method for the Quantification of Allopurinol and Lesinurad in Bulk and Pharmaceutical Formulations

2020 ◽  
Vol 5 (1) ◽  
pp. 51-55
Author(s):  
K.V. Ramanjaneyulu ◽  
K. Venkata Ramana ◽  
M. Prasada Rao
Keyword(s):  
Degradation Products ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Forced Degradation ◽  
Analysis Method ◽  
Degradation Study ◽  
Stability Indicating ◽  
Stress Study ◽  
Isocratic Hplc ◽  
Bulk Drug

The objective of this study was to develop and validate a method for simultaneous quantitative analysis of allopurinol and lesinurad in bulk drug and pharmaceutical formulations. An isocratic HPLC analysis method using a reverse phase Waters spherisorb ODS1 C18 column (250 mm × 4.6 mm, 5 μ) and a simple mobile phase without buffer was developed, optimized and fully validated. Analyses were carried out at a flow rate of 0.9 mL/min at 50 °C and monitored at 246 nm. This HPLC method exhibited good linearity, accuracy and selectivity. The recovery (accuracy) of both allopurinol and lesinurad from all matrices was greater than 98 %. The allopurinol and lesinurad peak detected in the samples of a forced degradation study and no interference of excepients or the degradation products formed during stress study. The method was rugged with good intra- and inter-day precision and sensitive. This stability indicating HPLC method was selective, accurate and precise for the simultaneous analysis of allopurinol and lesinurad in pharmaceutical formulations.

scholarly journals A SIMPLE (HPLC–UV) METHOD FOR THE QUANTIFICATION OF COLCHICINE IN BULK AND ETHOSOMAL GEL NANO-FORMULATION AND ITS VALIDATION

2017 ◽  
Vol 9 (7) ◽  
pp. 72 ◽  
Author(s):  
Ibrahim M. Abdulbaqi ◽  
Yusrida Darwis ◽  
Nurzalina Abdul Karim Khan ◽  
Reem Abou Assi ◽  
Gabriel Onn Kit Loh
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Reversed Phase ◽  
Hplc Method ◽  
Acid Oxidation ◽  
Limit Of Quantification ◽  
Stability Indicating ◽  
Stress Degradation

Objective: To develop and validate a stability-indicating reversed phase high-performance liquid chromatography (RP-HPLC) method for the determination of colchicine in bulk and ethosomal gel nano-formulation.Methods: The chromatographic conditions were optimized using stainless steel Hypersil Gold C-18 analytical column with the dimensions of 250 mm x 4.6 mm ID x 5 µm. The mobile phase consisted of acetonitrile and ammonium acetate buffer (20 mmol/l, pH=4.85) in the ratio of 32:68 v/v. The flow rate was set at 1 ml/min and the detection wavelength was 353 nm. The column was maintained at 30 °C and the injection volume was 10 µl. The stability of colchicine in different conditions was investigated by exposing the drug to stress degradation using acid, base, oxidation, heat and light.Results: There was no interference from excipients, impurities, dissolution media or degradation products at the retention time of colchicine 5.9 min indicating the specificity of the method. The limit of detection (LOD) and the limit of quantification (LOQ) were 8.64 ng/ml and 26.17 ng/ml respectively. The drug showed good stability under heat, acid, oxidation and light, but substantial degradation was observed under alkali condition. The procedure was validated for specificity, linearity, accuracy and precision.Conclusion: A simple, rapid, specific and stability-indicating HPLC–UV method for the determination of colchicine in the pure and ethosomal gel was successfully developed. The developed method was statistically confirmed to be accurate, precise, and reproducible.

scholarly journals SIMPLE QUANTIFIED AND VALIDATED STABILITY INDICATING STRESS DEGRADATION STUDIES OF ORAL ANTI-DIABETIC AGENT DAPAGLIFLOZIN BY RP-HPLC METHOD

2022 ◽  
pp. 231-237
Author(s):  
ARULSELVAN MURUGESAN ◽  
MUKTHINUTHALAPATI MATHRUSRI ANNAPURNA
Keyword(s):  
Dosage Form ◽  
Degradation Products ◽  
Active Pharmaceutical Ingredient ◽  
Hplc Method ◽  
Reverse Phase ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Stress Degradation

Objective: This method is focused on developing a precisely simplified and more accurate Reverse Phase–High Pressure Liquid Chromatography (RP-HPLC) method for the determination of Dapagliflozin in bulk and pharmaceutical dosage form as per guidelines of International Council for Harmonization (ICH). Methods: Evaluation and validation carried out using the RP-HPLC ZORBAX (C18) column (250 x 4.6 mm, 5 μm particle size) with a mobile phase consisting of Phosphate Buffer: Acetonitrile: Methanol in a ratio of 55:40:05 (v/v/v) at a flow rate of 1 ml/min with an injection volume of 10 μl. Results: Dapagliflozin was eluted at 2.12±0.05 min and detected at 225 nm. The regression equation y = 55762 x-29679 found to be linear with correlation coefficient r2 value of 0.9997. The developed RP-HPLC method was conveniently validated as per the ICH guidelines and found method was robust, sensitive, accurate, selective, specific, precise and linear. Conclusion: The proposed method was found to be accurate, precise, and robust for API and pharmaceutical dosage form as per experimentation analysis. The above developed method was found to be satisfied for Active Pharmaceutical Ingredient (API) and pharmaceutical formulation of Dapagliflozin to study its degradation products.

scholarly journals Development of Stability Indicating and Robust RP-HPLC Method for Determination of Teneligliptin

2018 ◽  
pp. 1-12
Author(s):  
Anvesha Vinit Ganorkar ◽  
Rekha S. Jibhkate ◽  
Krishna Radheshyam Gupta
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Hplc Method ◽  
Reverse Phase Hplc ◽  
Degradation Study ◽  
Ich Guidelines ◽  
Purity Analysis ◽  
Burman Design ◽  
Plackett Burman Design

A simple and rapid reverse-phase HPLC method was developed for determination of Teneligliptin (TGP) in the presence of its degradation products generated from forced decomposition studies. The HPLC separation was achieved on a C18 ACE column (150x 4.6 mm i.d.; 5 μm) using mobile phase as a mixture of Phosphate buffer pH-7.2 using ortho-phosphoric acid: methanol (30:70v/v). The UV detection was carried out at 245nm at ambient temperature and the flow rate of 1.0 mL/min. The calibration curve was found to be linear in the concentration range of 10-50 μg/mL(r=0.9993). Force degradation study was performed under various conditions like acidic, alkaline, oxidative, photolytic and mass balance calculations were carried out from the degradation results. The developed method was validated as per ICH guidelines with respect to linearity, accuracy, precision, limit of detection and quantification. The robustness of the proposed method was evaluated by the Plackett Burman design. The purity of the degraded sample was checked by peak purity analysis. The peaks of degradation products did not interfere with that of pure Teneligliptin.

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 A Selective High-Performance Liquid Chromatography Method for the Determination of Reboxetine in Bulk Drug and Tablets

2006 ◽  
Vol 89 (6) ◽  
pp. 1552-1556
Author(s):  
ArmaĞan Önal ◽  
Olcay SaĞiri ◽  
S Müge Çetin ◽  
Sidika Toker
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Depressive Disorders ◽  
Degradation Products ◽  
Severe Depression ◽  
Hplc Method ◽  
Chromatography Method ◽  
Relative Standard

Abstract Reboxetine is used as a selective noradrenaline reuptake inhibitor for the treatment of major depressive disorders. It is effective in the treatment of severe depression and safer to use than traditional tricyclic antidepressants. In this study, a novel, simple, and rapid stability-indicating high-performance liquid chromatography (HPLC) method for reboxetine methansulfonate was successfully developed and validated for the assay of tablets. The method was used to quantify reboxetine in tablets; it employed a C18 column (150 4.6 mm id) with an isocratic mobile phase consisting of methanolphosphate buffer (pH 7, 0.02 M; 55 + 45, v/v) at a flow rate of 1.0 μmL/min. Reboxetine was detected by an ultraviolet detector at 277 nm. The retention time of reboxetine was about 4.5 min. The developed HPLC method was validated with respect to linearity, precision, sensitivity, accuracy, and selectivity. The method was linear over the concentration range 150 g/mL (r 0.9999). The limits of detection and the quantitation of reboxetine were 0.1 and 0.3 μg/mL, respectively. The relative standard deviation values for intraday and interday precision were 0.781.01 and 1.081.37%, respectively. Selectivity was validated by subjecting a stock solution of reboxetine to neutral, acid, and alkali hydrolysis, as well as oxidation, dry heat treatment, and photodegradation. The peaks of the degradation products did not interfere with the peak of reboxetine. The results indicated that the proposed method could be used in a stability assay. The proposed method was successfully applied to the determination of reboxetine in tablets. Excipients present in the tablets did not interfere with the analysis.

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