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.

Identification, Characterization, and Quantification of Impurities of Safinamide Mesilate: Process-Related Impurities and Degradation Products

2017 ◽  
Vol 100 (4) ◽  
pp. 1029-1037 ◽  
Author(s):  
Liang Zou ◽  
Lili Sun ◽  
Hui Zhang ◽  
Wenkai Hui ◽  
Qiaogen Zou ◽  
...  
Keyword(s):  
Degradation Products ◽  
Hplc Method ◽  
Formation Mechanisms ◽  
Stability Indicating ◽  
Related Impurities ◽  
Related Substances ◽  
Water Ph ◽  
Bulk Drug ◽  
First Time

Abstract The characterization of process-related impurities and degradation products of safinamide mesilate (SAFM) in bulk drug and a stability-indicating HPLC method for the separation and quantification of all the impurities were investigated. Four process-related impurities (Imp-B, Imp-C, Imp-D, and Imp-E) were found in the SAFM bulk drug. Five degradation products (Imp-A, Imp-C, Imp-D, Imp-E, and Imp-F) were observed in SAFM under oxidative conditions. Imp-C, Imp-D, and Imp-E were also degradation products and process-related impurities. Remarkably, one new compound, identified as (S)-2-[4-(3-fluoro-benzyloxy) benzamido] propanamide (i.e., Imp-D), is being reported here as an impurity for the first time. Furthermore, the structures of the aforementioned impurities were characterized and confirmed via IR, NMR, and MS techniques, and the most probable formation mechanisms of all impurities proposed according to the synthesis route. Optimum separation was achieved on an Inertsil ODS-3 column (250 × 4.6 mm, 5 μm), using 0.1% formic acid in water (pH adjusted to 5.0) and acetonitrile as the mobile phase in gradient mode. The proposed method was found to be stability-indicating, precise, linear, accurate, sensitive, and robust for the quantitation of SAFM and its process-related substances, including its degradation products.

scholarly journals Stability Indicating HPLC Determination of Risperidone in Bulk Drug and Pharmaceutical Formulations

2011 ◽  
Vol 2011 ◽  
pp. 1-6 ◽  
Author(s):  
Zarna R. Dedania ◽  
Ronak R. Dedania ◽  
Navin R. Sheth ◽  
Jigar B. Patel ◽  
Bhavna Patel
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Pharmaceutical Formulations ◽  
Assay Method ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Stress Studies ◽  
Liquid Chromatographic Separation ◽  
Bulk Drug ◽  
Liquid Chromatographic

The objective of the current study was to develop a validated stability-indicating assay method (SIAM) for risperidone after subjecting it to forced decomposition under hydrolysis, oxidation, photolysis, and thermal stress conditions. The liquid chromatographic separation was achieved isocratically on a symmetry C18 column (5 μm size, 250 mm × 4.6 mm i.d.) using a mobile phase containing methanol: acetonitrile (80 : 20, v/v) at a flow rate of 1 mL/min and UV detection at 280 nm. Retention time of risperidone was found to be . The method was linear over the concentration range of 10–60 μg/mL with a limit of detection and quantitation of 1.79 and 5.44 μg/mL, respectively. The method has the requisite accuracy, specificity, sensitivity, and precision to assay risperidone in bulk form and pharmaceutical dosage forms. Degradation products resulting from the stress studies did not interfere with the detection of Risperidone, and the assay is thus stability indicating.

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. 

A Novel Stability Indicating RP-HPLC Method Development and Validation for Simultaneous Estimation of Bictegravir, Emtricitabine and Tenofovir in Pure and Fixed Dose Combination

2019 ◽  
Vol 4 (1) ◽  
pp. 7-13
Author(s):  
G. Vijay Swaroop Singh ◽  
T.E. Divakar
Keyword(s):  
Method Development ◽  
Sodium Perchlorate ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Fixed Dose ◽  
Simultaneous Estimation ◽  
Stability Indicating ◽  
Stress Degradation ◽  
Dose Combination ◽  
Bulk Drug

A novel, simple, precise, accurate stability indicating liquid chromato-graphy method was developed for the separation and simultaneous quantification of bictegravir, emtricitabine, tenofovir in bulk drug and pharmaceutical formulations. Separation was achieved on ProntoSILHypersorb ODS C18 column using mobile phase of 0.1 M sodium perchlorate, methanol in the ratio of 65:35 (v/v), pH 4.8 at a flow rate of 1.0 mL/min and UV detection was monitored at a wavelength of 258 nm. In these conditions, well resolved peaks were observed with acceptable system suitability at a retention time of 4.6 min for bictegravir, 7.0 min for emtricitabine and 10.1 min for tenofovir. Very high correlated linearity range was found to be 5-30 μg/mL for bictegravir, 20-120 μg/mL for emtricitabine and 2.5-15 μg/mL for tenofovir. The method can separate and identify the unknown degradation compounds formed during stress degradation study.

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 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.

scholarly journals Validated stability-indicating method for estimation of related substances of paroxetine in active pharmaceutical ingredient and its pharmaceutical dosage forms

2020 ◽  
Vol 11 (4) ◽  
pp. 8004-8011
Author(s):  
Surapuraju Pavan Kumar Raju ◽  
Raveendra Reddy J
Keyword(s):  
Mobile Phase ◽  
Method Development ◽  
Degradation Products ◽  
Drug Stability ◽  
Active Pharmaceutical Ingredient ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Stress Studies ◽  
Related Substances ◽  
Stability Indicating Method

Validated stability-indicating analytical method was established for the quantitative determination of paroxetine and its related substances in API and it’s finished product in the presence of degradation products. To prove the stability-indicating nature of the method, stress studies were carried out. The method was developed by using (Waters, symmetry C18, 250×4.6 mm, 5 μm column) employing water:THF: TFA 90:10:1 (v/v/v) as mobile phase-A and mobile phase-B consist of ACN:THF: TFA the proportion of 90:10:1 (v/v/v) in a gradient mode with a flow rate of 1.5 mL/min was chosen. The column and sample cooler were kept at 45°C and 5°C respectively and 285 nm used as detection wavelength. Significant degradation observed in alkaline conditions, whereas no signification decay in drug stability was observed in other decomposition environments. Method development as well as optimisation studies were done by analysing the samples generated in the stress studies and spiked samples. Mass balance was found to be in the range of 90.3 and 100.1%, signifying the method is stability-indicating. All earlier analysis methods for the analysis of paroxetine have not been entirely validated by considering all the degradation products. The established method validated as per ICH Q2 (R1) and considered as linear, specific, accurate, precise, rugged, robust and found to be suitable for the routine and stability analysis of the product.

Development and Validation of a Stability-Indicating HPLC Method for Imidapril and Its Degradation Products Using a Design of Experiment (DoE) Approach

2017 ◽  
Vol 100 (6) ◽  
pp. 1727-1738 ◽  
Author(s):  
Abiramasundari Arumugam ◽  
Amita Joshi ◽  
Kamala K Vasu
Keyword(s):  
Flow Rate ◽  
Design Of Experiment ◽  
Degradation Products ◽  
Desirability Function ◽  
Hplc Method ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Two Factors ◽  
Derringer’S Desirability Function ◽  
Imidapril Hydrochloride

Abstract The present work focused on the application of design of experiment (DoE) principles to the development and optimization of a stability-indicating method (SIM) for the drug imidapril hydrochloride and its degradation products (DPs). The resolution of peaks for the DPs and their drug in a SIM can be influenced by many factors. The factors studied here were pH, gradient time, organic modifier, flow rate, molar concentration of the buffer, and wavelength, with the aid of a Plackett–Burman design. Results from the Plackett–Burman study conspicuously showed influence of two factors, pH and gradient time, on the analyzed response, particularly, the resolution of the closely eluting DPs (DP-5 and DP-6) and the retention time of the last peak. Optimization of the multiresponse processes was achieved through Derringer’s desirability function with the assistance of a full factorial design. Separation was achieved using a C18 Phenomenex Luna column (250 × 4.6 mm id, 5 µm particle size) at a flow rate of 0.8 mL/min at 210 nm. The optimized mobile phase composition was ammonium–acetate buffer (pH 5) in pump A and acetonitrile–methanol (in equal ratio) in pump B with a run time of 40 min using a gradient method.

scholarly journals Development and Validation of a Stability-Indicating RP-HPLC Method for Determination of Atomoxetine Hydrochloride in Tablets

2010 ◽  
Vol 93 (4) ◽  
pp. 1207-1214 ◽  
Author(s):  
Sejal K Patel ◽  
Natvarlal J Patel
Keyword(s):  
Degradation Products ◽  
Hplc Method ◽  
Stress Conditions ◽  
Acid Base ◽  
Photodiode Array Detection ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Rp Hplc ◽  
Wet Heat

Abstract This paper describes the development of a stability-indicating RP-HPLC method for the determination of atomoxetine hydrochloride (ATX) in the presence of its degradation products generated from forced decomposition studies. The drug substance was subjected to stress conditions of acid, base, oxidation, wet heat, dry heat, and photodegradation. In stability tests, the drug was susceptible to acid, base, oxidation, and dry and wet heat degradation. It was found to be stable under the photolytic conditions tested. The drug was successfully separated from the degradation products formed under stress conditions on a Phenomenex C18 column (250 4.6 mm id, 5 m particle size) by using acetonitrilemethanol0.032 M ammonium acetate (55 + 05 + 40, v/v/v) as the mobile phase at 1.0 mL/min and 40C. Photodiode array detection at 275 nm was used for quantitation after RP-HPLC over the concentration range of 0.55 g/mL with a mean recovery of 100.8 0.4 for ATX. Statistical analysis demonstrated that the method is repeatable, specific, and accurate for the estimation of ATX. Because the method effectively separates the drug from its degradation products, it can be used as a stability-indicating method.

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