scholarly journals Development and Validation of Stability Indicating LC-PDA Method for Mycophenolate Mofetil in Presence of Mycophenolic Acid and Its Application for Degradation Kinetics and pH Profile Study

2014 ◽  
Vol 2014 ◽  
pp. 1-9 ◽  
Author(s):  
Vishnu P. Choudhari ◽  
Anna Pratima G. Nikalje
Keyword(s):  
Mycophenolate Mofetil ◽  
Degradation Products ◽  
Degradation Kinetics ◽  
Oxidative Degradation ◽  
Reversed Phase ◽  
Hplc Method ◽  
Design Tool ◽  
Ph Profile ◽  
Stability Indicating ◽  
Specificity And Sensitivity

Factorial design tool applied for development of isocratic reversed-phase stability-indicating HPLC method for the analysis of mycophenolate mofetil (MMF) and its degradation products. MMF stress degradation products mycophenolate acid (MPA) and DP3 (USP impurity H) were isolated and used for quantitation. Separation achieved on a Symmetry C18 (250 mm × 4.6 mm, 5.0 μ) column using a methanol: acetate buffer (75 : 25 v/v), pH 6.0 (adjusted with acetic acid), at 0.5 mL flow rate, column maintained at 55°C, and data integrated at 251 nm. MMF is subjected to hydrolysis, oxidation, heat degradation, and so forth; under all these conditions degraded products are well separated. The method validation characteristics included accuracy, precision, linearity, range, specificity, and sensitivity. Robustness testing is conducted to evaluate the effect of minor changes to the chromatographic conditions and to establish appropriate system suitability parameters. The proposed method is used to investigate kinetics of acid, alkali hydrolysis and oxidation process. Major degradation products MPA and DP3 were isolated and quantitated. Characterization of MPA by NMR and LC-MS/MS and other degraded products by LC-MS/MS is attempted successfully. The method is used successfully for the quality assessment of three MMF drug commercial formations and its acid, alkali, and oxidative degradation kinetics study.

scholarly journals Stress Degradation Studies on Bimatoprost and Development of Validated Stability Indicating Densitometric RP-TLC and HPLC Methods

2019 ◽  
pp. 5-10
Author(s):  
Maha M Abou El-Alamin ◽  
Safaa Toubar ◽  
Maha A Elabd ◽  
Nahla N Salama ◽  
Mohammed Walash
Keyword(s):  
Degradation Products ◽  
Research Work ◽  
Oxidative Degradation ◽  
Ophthalmic Solution ◽  
Reversed Phase ◽  
Hplc Method ◽  
Stability Studies ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Stress Degradation

Simple, sensitive and accurate stability-indicating densitometric RP-TLC and RP HPLC-UV methods were developed and validated for analysis of Bimatoprost (BMT). Stress stability studies were performed using hydrolytic (acid & alkai) and oxidative degradation products and conformed using LC-MS. Structure elucidation and pathway of degradation were presented. Both methods were based on reversed phase thin-layer and liquid chromatographic separation of BMT from hydrolytic and oxidative degradation products. Acetonitrile, water and 33% ammonia (4:5:1, by volume) and acetonitrile –water (40:60, v/v) at 30◦C were used as mobile phases for separation of BMT from degradation products using RP TLC and HPLC methods respectively. Quantification was achieved at 220 nm for both methods. The linear ranges were 0.5-6.0 μg/band and 5 – 100 μg /mL with mean recoveries ± RSD%, of 98.72 ± 0. 31% and 99.25 ± 0.59% for the two methods respectively. The specificity of HPLC method was further assured by peak purity. The proposed methods are rapid with retention time less than 6 min. The methods met ICH regulatory requirements. The two methods were successfully applied for the quantification of BMT in drug substance and ophthalmic solution with acceptable accuracy and precisions; the label claim percentages were 93.145 ± 0.89 and 95.35 + 0.65 for densitometric RP-TLC and RP HPLC-UV methods respectively. The research work has a great value for quality control and stability studies of BMT.

scholarly journals Validated Stability Indicating Chromatographic Methods for Quantification of Imidocarb Dipropionate; Application for the Determination of Its Residues in Bovine Meat and Milk Samples

2020 ◽  
Vol 103 (4) ◽  
pp. 980-988
Author(s):  
Ghada AbdElHamid Sedik ◽  
Doha Mohamed Naguib ◽  
Fahima Morsy ◽  
Hala Elsayed Zaazaa
Keyword(s):  
Degradation Products ◽  
Reversed Phase ◽  
Hplc Method ◽  
Stability Indicating ◽  
Milk Samples ◽  
Chromatographic Methods ◽  
Ich Guidelines ◽  
Imidocarb Dipropionate ◽  
Tlc Plates

Abstract Background Imidocarb dipropionate (IMD) is an immunomodulator agent commonly used for treatment of anaplasmosis in cattle. Objective Thus, two sensitive, specific, and precise stability-indicating chromatographic methods have been developed, optimized, and validated for its determination in presence of its acid, alkaline, and oxidative stressed degradation products. Method The first method is based on separation of IMD and its forced induced degradation products on reversed phase cyano column using isocratic elution system consisted of sodium acetate buffer–methanol–acetonitrile (55: 30:15, v/v/v), pH 4.6 at a flow rate of 1.2 mL/min, and UV detection at 254 nm. The second method utilized TLC combined with densitometric determination of the separated bands at 254 nm. The separation was achieved using silica gel 60 F254 TLC plates with a mixture of ethyl acetate–methanol–ammonia–water (8.5:1:0.5:0.2, v/v/v/v) as a developing system. Results HPLC analysis was applied in range of 0.25–40 µg/mL with LOD of 0.073 µg/mL. While densitometric measurements showed linearity in the range of 0.1–1.8 µg/band with LOD of 0.02 µg/band. Conclusions The suggested methods were validated in compliance with the ICH guidelines and were successfully applied for determination of IMD in its commercial veterinary formulations with good recoveries. Furthermore, the proposed HPLC method was extended to the determination of IMD residues in bovine meat and milk samples Highlights Bovine meat, HPLC, Imidocarb dipropionate, Milk, TLC.

Development and Validation of Stability-Indicating HPLC Method for Roflumilast and Related Substances

2013 ◽  
Vol 781-784 ◽  
pp. 68-71 ◽  
Author(s):  
Fang Tan
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Reversed Phase ◽  
Hplc Method ◽  
Forced Degradation ◽  
Dihydrogen Phosphate ◽  
Column Temperature ◽  
Stability Indicating ◽  
Related Substances ◽  
Limit Of Quantitation

A reversed phase HPLC method was developed and validated for analysis of roflumilast, its related substances and degradation products, using Ecosil C18 column (250×4.6 mm, 5 μm) with a flow rate of 1.0 ml/min and detection wavelength of 215nm. The mobile phase was a mixture of acetonitrile and 0.005mol·L-1ammonium dihydrogen phosphate buffer pH 3.5 in the ratio of 48:52 (v/v). The samples were analyzed using 20 μl injection volume and the column temperature was maintained at 30°C. The limit of detection and limit of quantitation were found to be 2.6 ng/ml and 8ng/ml, respectively. The stability-indicating capability of method was established by forced degradation studies and method demonstrated successful separation of drug, its related substances and degradation products. The method is sensitive, specific, accurate, precise and stability indicating for the quantitation of drug, its related substances and other degradation compounds.

scholarly journals Development and validation by statistical treatment of stability indicating RP-HPLC method for quantification of Orlistat in Orlistat-loaded solid dispersion

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Kiran Singh Sharma ◽  
Jagannath Sahoo
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Solid Dispersions ◽  
Statistical Treatment ◽  
Reversed Phase ◽  
Hplc Method ◽  
Statistical Parameters ◽  
Analytical Technique ◽  
Stability Indicating ◽  
Limit Of Quantitation

Abstract Background Most of the analytical methods reported for the estimation of Orlistat were complex, expensive, and deficient in reproducibility with no or very less informative regarding various statistical methods and equations used for the validation purpose. This study provides a fast, accurate, descriptive, and precise isocratic reversed phase high-performance liquid chromatographic (HPLC) method using Waters Spherisorb 5 μm Octadecyl-silica-2 (250 × 4.6 mm) column, for the estimation of Orlistat in bulk drug and pharmaceutical formulations with minimized drug extraction steps. The drug was detected in an analytical column with mobile phase comprising a mixture of methanol, acetonitrile, and 2% phosphoric acid in the ratio of 85:14:1 v/v/v at flow rate of 1 ml/min with elution monitoring at 215.0 nm. Results The retention time for Orlistat was found to be 5.9 min with sharp and proper peak. The linearity was covered over the concentration range of 1.00–10.00 μg/ml (r2 = 0.9997) with a limit of detection and limit of quantitation 0.06 and 0.2 μg/ml, respectively. The developed analytical technique was found to be validated for all the parameters within the acceptance criteria of ICH guidelines. The mean ± standard deviation (SD) recoveries of Orlistat were 99.87 ± 0.45. Conclusion The optimized method was well precise, accurate, sensitive, stability indicating, and tested with all statistical parameters. Thus, the method can be conveniently used in quality control and routine analysis of Orlistat containing solid dispersions and other formulations. The main advantage of the developed method was its high specificity for the estimation of Orlistat in presence of various degradation products resulting from stress conditions and formulation excipients.

scholarly journals Stability Indicating HPLC Method for the Determination of Delamanid in Pharmaceutical Dosage Form

2021 ◽  
Vol 11 (1-s) ◽  
pp. 108-112
Author(s):  
Advaita B. Patel ◽  
Deepa R. Patel ◽  
Dhaval M. Patel ◽  
Mansi Babaria
Keyword(s):  
Analytical Method ◽  
Mobile Phase ◽  
Dosage Form ◽  
Degradation Products ◽  
Stress Test ◽  
Reversed Phase ◽  
Hplc Method ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating

Delamanid is successfully used for treatment of MDR TB. A stability indicating analytical method has been developed and validated. In this study Delamanid was degraded under different stress test conditions as per International Conference on Harmonization. The degraded samples were used to develop a stability-indicating high performance liquid chromatographic (HPLC) method for the Delamanid. The Delamanid was well separated from degradation products using a reversed-phase Hypersil BDS C18 (250 mm × 4.6mm i.d., 5µm) column and a mobile phase comprising of 0.01M pH 2.70 Phosphate Buffer: Acetonitrile (pH 3.50) 70:30, pH of mobile phase was adjusted with Glacial acetic acid and other HPLC parameters were flow rate 1 mL/min, detection wavelength 254 nm and injection volume 10 µl. The method was validated for linearity, precision, accuracy, ruggedness and robustness. Results obtained after validation study indicating that the proposed single method allowed analysis of Delamanid in the presence of their degradation products formed under a variety of stress conditions. The developed procedure was also applicable to the determination of stability of the Delamanid in commercial pharmaceutical dosage form. Keywords:  Delamanid, stability indicating analytical method, HPLC

scholarly journals Stability-indicating RP-HPLC method for determination of beclomethasone dipropionate in nanocapsule suspensions

2015 ◽  
Vol 51 (4) ◽  
pp. 803-810 ◽  
Author(s):  
Janaíne Micheli Chassot ◽  
Luana Mota Ferreira ◽  
Felipe Pereira Gomes ◽  
Letícia Cruz ◽  
Leandro Tasso
Keyword(s):  
Mobile Phase ◽  
Beclomethasone Dipropionate ◽  
Degradation Products ◽  
Degradation Kinetics ◽  
Hplc Method ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Relative Standard ◽  
Bulk Drug

abstract A simple stability-indicating RP-HPLC/UV method was validated for determination of beclomethasone dipropionate (BD) in nanocapsule suspensions. Chromatographic conditions consisted of a RP C18column (250 mm x 4.60 mm, 5 µm, 110 Å), using methanol and water (85:15 v/v) as mobile phase at 1.0 mL/min with UV detection at 254 nm. The calibration curve was found to be linear in the concentration range of 5.0-25.0 µg/mL with a correlation coefficient > 0.999. Precision was demonstrated by a relative standard deviation lower than 2.0%. Accuracy was assessed by the recovery test of BD from nanocapsules (98.03% to 100.35%). Specificity showed no interference from the components of nanocapsules or from the degradation products derived from acid, basic and photolytic conditions. In conclusion, the method is suitable to be applied to assay BD in bulk drug and in nanocapsules, and it can be employed to study stability and degradation kinetics.

Stability-Indicating RP-HPLC and CE Methods for Simultaneous Determination of Bisoprolol and Perindopril in Pharmaceutical Formulation: A Comparative Study

2020 ◽  
Vol 58 (8) ◽  
pp. 747-758
Author(s):  
Said A Hassan ◽  
Nancy W Nashat ◽  
Mohamed R Elghobashy ◽  
Samah S Abbas ◽  
Azza A Moustafa
Keyword(s):  
Capillary Electrophoresis ◽  
Simultaneous Determination ◽  
High Performance ◽  
Degradation Products ◽  
Reversed Phase ◽  
Hplc Method ◽  
Pharmaceutical Formulation ◽  
British Pharmacopoeia ◽  
Stability Indicating

Abstract Two fast, accurate and selective stability-indicating methods were developed and validated for the simultaneous determination of bisoprolol, perindopril and three of their possible degradation products. The first proposed method was a gradient reversed phase-high-performance liquid chromatography (HPLC) method, whereas the second was a capillary electrophoresis method. The structures of the obtained degradation products were elucidated using infrared and mass spectrometry. They were also confirmed to be either a drug impurity in the British Pharmacopoeia or a precursor to such impurity. The linearity for bisoprolol and perindopril was achieved in the range of 1–20 μg mL−1 and 5–30 μg mL−1 for HPLC and capillary electrophoresis methods, respectively. The proposed methods were validated according to the International Conference on Harmonisation guidelines. The HPLC method proved to be more sensitive and succeeded in the quantitative determination of the obtained degradation products. Also, it was able to quantify perindopril impurity up to three times lower than the desired limit set by the British Pharmacopoeia. They were successfully employed in the determination of bisoprolol and perindopril in their combined pharmaceutical formulation.

Validated Stability−Indicating LC Method for Estimation of Amoxicillin Trihydrate in Pharmaceutical Dosage Forms and Time-Dependent Release Formulations

2011 ◽  
Vol 4 (2) ◽  
pp. 1423-1427 ◽  
Author(s):  
Sarwar Beg ◽  
S M Hasnain ◽  
S Swain ◽  
K Kohli
Keyword(s):  
Degradation Products ◽  
Degradation Kinetics ◽  
Pharmaceutical Formulations ◽  
Time Dependent ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Specificity And Sensitivity ◽  
Stress Degradation ◽  
Amoxicillin Trihydrate ◽  
Bulk Drug

The objective of this study was to establish a validated stability-indicating LC method for routine analysis of amoxicillin trihydrate in bulk drug samples, different pharmaceutical formulations, and degradation kinetics of the drug under different ICH recommended stress conditions. Chromatographic separation was achieved by a Capacel Pak C18 column with 50:50% v/v methanol-0.02 M phosphate buffer as mobile phase having pH 3.5 and flow rate of 1.0 ml/min; with UV absorbance at 229 nm. The method was validated for system suitability, linearity, precision, accuracy, robustness, specificity and sensitivity. The drug was subjected to stress degradation by exposure to acid and alkaline hydrolysis, oxidation, and photodegradation. It was observed that peaks of all degradation products were well resolved from the pure drug with significantly different retention times, which indicated the specificity and stability-indicating properties of the method. When the utility of the method was verified by analysis of the drug in marketed formulations and in-house time-dependent release tablet formulations, the assay was found to be 99.6–100.4%. Statistical analysis proves that the method is repeatable, selective, and accurate for the estimation of amoxicillin trihydrate in bulk drug samples and also 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.

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