Stress Degradation Studies of Anagliptin, Development of Validated Stability Indicating Method, Degradation Kinetics Study, Identification and Isolation of Degradation Products

2018 ◽  
Vol 81 (11) ◽  
pp. 1533-1550
Author(s):  
Charu P. Pandya ◽  
Sadhana J. Rajput
Keyword(s):  
Degradation Products ◽  
Degradation Kinetics ◽  
Kinetics Study ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Stress Degradation ◽  
Degradation Studies

Development and Validation of a Stability-Indicating HPLC-Photodiode Array Detector Method for Formulation Analysis and Degradation Kinetics and Dissolution Studies of Mycophenolate Sodium and HPLC/MS/MS Characterization of its Stress Degradation Products

2013 ◽  
Vol 96 (3) ◽  
pp. 593-598
Author(s):  
Anna Pratima G Nikalje ◽  
Vishnu P Choudhari
Keyword(s):  
Degradation Product ◽  
Degradation Products ◽  
Degradation Kinetics ◽  
Array Detector ◽  
Forced Degradation ◽  
Product Analysis ◽  
Mycophenolate Sodium ◽  
Stability Indicating ◽  
Stress Degradation

Abstract A simple stability-indicating isocratic RP-HPLC method was developed and validated for the determination of mycophenolate sodium and its alkali degradation product. Forced degradation of the drug was carried out under thermolytic, photolytic, acid/base hydrolytic, and oxidative stress conditions. Alkali degradation product DP1 was isolated, and separation of stress degradation products was achieved on a Symmetry C18 (250 × 4.6 mm × 5.0 μm) column using the mobile phase methanol–acetate buffer adjusted with acetic acid to pH 6.0 (76 + 24, v/v) at a 0.55 mL/min flow rate and 50°C. Data were integrated at the detection wavelength of 251 nm. The method validation characteristics included accuracy, precision, linearity, range, specificity, and sensitivity per International Conference on Harmonization guidelines. Robustness testing was conducted to evaluate the effect of minor changes in the chromatographic conditions and to establish appropriate system suitability parameters. Structural elucidation of degraded products was performed by HPLC/MS/MS. The method was used successfully for drug product analysis, dissolution study, and determination of the drug's acid, alkali, and oxidative degradation kinetics.

STABILITY INDICATING RP-HPLC METHOD FOR SEPARATION AND QUANTIFICATION OF RELATED SUBSTANCES OF TICLOPIDINE IN BULK AND PHARMACEUTICAL FORMULATIONS

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (08) ◽  
pp. 75-78
Author(s):  
B. S. Venkateswarlu ◽  
Prudhvi N. Sai ◽  
Keyword(s):  
Degradation Products ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Standard Drug ◽  
Stability Indicating ◽  
Stress Studies ◽  
Related Substances ◽  
Stability Indicating Method ◽  
Stress Degradation ◽  
Bulk Drug

A simple, specific, accurate and stable reverse phase liquid chromatographic method was developed for the simultaneous determination of ticlopidine and its related impurities A and B in bulk drug and tablet dosage forms. The analysis has been performed on XTerra C18 column (250 mm×4.6 mm; 5 µ id) and mobile phase containing of methanol and pH 6.8 phosphate buffer in the ratio of 80:20 (V/V). The detection was carried at 228 nm with a flow rate of 1.0 mL/min. The retention times were found to be 8.9, 5.98 and 4.62 min for ticlopidine, impurities A and B, respectively. The method was validated according to ICH guidelines. The method was validated for specificity, precision, linearity, accuracy and robustness. The linearity range of 50-200 µg/mL for ticlopidine and 0.5-2.0 µg/mL for impurity A and B. The recoveries of ticlopidine and impurities were found to be within the range of 98-102 and the % RSD in each spiked level was found to be less than 2. The stress degradation studies confirmed that the method was effectively separate the degradation products and impurities formed in the stress studies and hence the method was found to be stability indicating method. The method can effectively quantify the standard drug ticlopidine and its impurities A and B in bulk drug and pharmaceutical formulations.

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 Optimization and Establishment of a Validated Stability-Indicating HPLC Method for Study of the Stress Degradation Behavior of Metoprolol Succinate

2010 ◽  
Vol 93 (3) ◽  
pp. 911-916 ◽  
Author(s):  
Mitesh D Phale ◽  
Purnima D Hamrapurkar
Keyword(s):  
Degradation Products ◽  
Hplc Method ◽  
Stress Conditions ◽  
Dihydrogen Phosphate ◽  
Sodium Dihydrogen Phosphate ◽  
Metoprolol Succinate ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Successful Separation ◽  
Stress Degradation

Abstract A stability-indicating HPLC method has been established for analysis of metoprolol succinate in the presence of products generated in a stress degradation study. The drug was subjected to stress conditions of hydrolysis, oxidation, photolysis, and thermal decomposition. Extensive degradation was found to occur in an alkaline medium and under thermal stress. Minimum degradation was observed in an acidic medium and under photolytic and oxidative stress. Successful separation of the drug from its degradation products formed under stress conditions was achieved on a C18 column using sodium dihydrogen phosphate bufferacetonitrile (70 + 30) mobile phase. The flow rate was 1 mL/min, and the detection wavelength was 274 nm. The method was validated for linearity, range, precision, accuracy, LOQ, and LOD. Because the method effectively separates the drugs from their degradation products, it can be used as a stability-indicating method.

STRESS DEGRADATION STUDIES ON HYDROCHLOROTHIAZIDE AND LISINOPRIL USING VALIDATED STABILITY INDICATING HIGH PERFORMANCE THIN LAYER CHROMATOGRAPHIC METHOD

INDIAN DRUGS ◽  
2017 ◽  
Vol 54 (04) ◽  
pp. 53-60
Author(s):  
K. G Patel ◽  
H. G. Rana ◽  
N. N Mistry ◽  
T. R Gandhi ◽  
Keyword(s):  
Thin Layer ◽  
High Performance ◽  
Chromatographic Method ◽  
Degradation Products ◽  
Phase System ◽  
Standard Drug ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Stress Degradation ◽  
Acidic Degradation

A specific stability indicating high-performance thin-layer chromatographic method for analysis of hydrochlorothiazide and lisinopril in formulations was developed and validated. The method employed precoated silica gel 60F254 HPTLC as the stationary phase. The optimized mobile phase system consisted of acetic acid: methanol: toluene (4:3:8, V/V/V), that gave compact spots for lisinopril and hydrochlorothiazide at Rf of 0.29 and 0.68, at 220 nm, respectively. The drugs were subjected to various accelerated conditions. The peaks of degraded products under various accelerated conditions were well resolved from the peak of standard drug with different Rf values and drug was more susceptible to acidic degradation. Linear relationship was found in the range of 800–1800 and 800-2300ng/band for hydrochlorothiazide and lisinopril respectively. Various parameters were validated as per ICH guideline. Moreover, the method could effectively separate the drug from its degradation products; hence it can be employed as a stability indicating method.

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