STABILITY-INDICATING UPLC METHOD FOR DETERMINATION OF RAMELTEON AND THEIR DEGRADATION PRODUCTS IN ACTIVE PHARMACEUTICAL INGREDIENTS

2012 ◽  
Vol 35 (5) ◽  
pp. 688-699 ◽  
Author(s):  
I. Ugandar Reddy ◽  
P. Nageswara Rao ◽  
V. Ranga Reddy ◽  
K. V. V. Satyanarayana
Keyword(s):  
Degradation Products ◽  
Active Pharmaceutical Ingredients ◽  
Stability Indicating ◽  
Pharmaceutical Ingredients

scholarly journals DEVELOPMENT AND VALIDATION OF STABILITY INDICATING RP-HPLC METHOD FOR THE SIMULTANEOUS ESTIMATION OF ETHINYL ESTRADIOL AND GESTODENE IN BULK AND PHARMACEUTICAL DOSAGE FORMS

2021 ◽  
pp. 49-58
Author(s):  
D. SUCHITRA ◽  
BATTU SATYANARAYANA
Keyword(s):  
Ethinyl Estradiol ◽  
Degradation Products ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Active Pharmaceutical Ingredients ◽  
Economic Stability ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Pharmaceutical Ingredients ◽  
Rp Hplc

Objective: The principal objective of this study is to develop and validate a simple, new, fast, selective, precise, and economic stability-indicating the RP-HPLC method for the simultaneous estimation of Ethinyl estradiol and Gestodene in a bulk and pharmaceutical dosage form. Methods: The present method was developed and validated on a Waters HPLC system using Phenomenex Gemini C18(250 mm × 4.6 mm i.d., 5 µm particle size) column and mobile phase composition of phosphate buffer: Acetonitrile (75:25 v/v) and the pH was adjusted to 3.6 using dilute orthophosphoric acid. The system was regulated at 1.0 ml/min flow rate at 237 nm UV detection. Results: The two drugs Ethinyl Estradiol and Gestodene, were eluted at 1.788 min and 3.475 min retention time, respectively. The analytical parameters such as accuracy, precision, linearity, LOD, LOQ, ruggedness, and robustness were used for validating the developed method according to International Conference on Harmonisation [ICH] guidelines. Linearity was exhibited over the concentration range of 10-50µg/ml and 25-125µg/ml for Ethinyl Estradiol and Gestodene, respectively. The method revealed the Limit of Detection and Quantitation values for Ethinyl Estradiol and Gestodene were 1.399µg/ml, 3.909µg/ml and 4.24µg/ml, 11.85µg/ml, respectively. The stress testing was carried out to give rise to degradation products by exposing the drugs to acid, alkali, thermal, oxidative, photolytic, and hydrolytic degradation. The obtained data showed that the content of Active pharmaceutical ingredients and the degradation products were successfully separated without any interference, which confirmed the stability-indicating nature of the developed method. Conclusion: The new, simple, rapid, selective, precise, and economic stability-indicating RP-HPLC method has been successfully developed and validated. It can be satisfactorily applied for the periodic laboratory quantitative estimation of Ethinyl Estradiol and Gestodene in formulations and active pharmaceutical ingredients.

scholarly journals Determination of Cefdinir by a Stability-Indicating Liquid Chromatographic Method

2005 ◽  
Vol 88 (6) ◽  
pp. 1661-1665 ◽  
Author(s):  
Tushar N Mehta ◽  
Gunta Subbaiah ◽  
Kilambi Pundarikakshudu
Keyword(s):  
Chromatographic Method ◽  
Degradation Products ◽  
Reversed Phase ◽  
Stability Indicating ◽  
Pharmaceutical Ingredients ◽  
Degraded Samples ◽  
Liquid Chromatographic Method ◽  
Phase Liquid ◽  
Liquid Chromatographic

Abstract A simple, fast, specific, stability-indicating, and precise reversed-phase liquid chromatographic method was developed for the determination of Cefdinir in its different dosage forms, i.e., capsules and suspensions. The method was developed and optimized by analyzing the placebo preparation, formulations, and degraded samples of the drug substance according to the International Conference on Harmonization. The proposed method can successfully separate the drug from degradation products formed under stress conditions along with pharmaceutical ingredients such as preservatives. The developed method was used successfully to determine Cefdinir in capsules and Insta-use suspensions. The developed method was found to be linear for a concentration range of 6–14 μg/mL. Average recoveries obtained with the method were 99.3 ± 0.4 and 99.6 ± 0.4% for Insta-use suspensions and capsules, respectively. The method was shown to be specific, precise, and robust.

Stability Indicating Liquid Chromatographic Method for the Determination of Fenofibrate and its Application to Kinetic Studies

2013 ◽  
Vol 5 (4) ◽  
pp. 1866-1874
Author(s):  
K. Srinivasa Rao ◽  
Keshar N K ◽  
N Jena ◽  
M.E.B Rao ◽  
A K Patnaik
Keyword(s):  
Degradation Products ◽  
Kinetic Studies ◽  
Pharmaceutical Formulations ◽  
Assay Method ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Zero Order Kinetics ◽  
Relative Standard ◽  
Liquid Chromatographic

A stability-indicating LC assay method was developed for the quantitative determination of fenofibrate (FFB) in pharmaceutical dosage form in the presence of its degradation products and kinetic determinations were evaluated in acidic, alkaline and peroxide degradation conditions. Chromatographic separation was achieved by use of Zorbax C18 column (250 × 4.0 mm, 5 μm). The mobile phase was established by mixing phosphate buffer (pH adjusted 3 with phosphoric acid) and acetonitrile (30:70 v/v). FFB degraded in acidic, alkaline and hydrogen peroxide conditions, while it was more stable in thermal and photolytic conditions. The described method was linear over a range of 1.0-500 μg/ml for determination of FFB (r= 0.9999). The precision was demonstrated by relative standard deviation (RSD) of intra-day (RSD= 0.56– 0.91) and inter-day studies (RSD= 1.47). The mean recovery was found to be 100.01%. The acid and alkaline degradations of FFB in 1M HCl and 1M NaOH solutions showed an apparent zero-order kinetics with rate constants 0.0736 and 0.0698  min−1 respectively and the peroxide degradation with 5% H2O2 demonstrated an apparent first-order kinetics with rate constant k = 0.0202 per min. The t1/2, t90   values are also determined for all the kinetic studies. The developed method was found to be simple, specific, robust, linear, precise, and accurate for the determination of FFB in pharmaceutical formulations.  

ICH/FDA Guidelines-Compliant Validated Stability-Indicating HPLC-UV Method for the Determination of Axitinib in Bulk and Dosage Forms

2020 ◽  
Vol 16 (8) ◽  
pp. 1106-1112
Author(s):  
Ibrahim A. Darwish ◽  
Nasr Y. Khalil ◽  
Mohammad AlZeer
Keyword(s):  
High Performance ◽  
Kinase Inhibitor ◽  
Degradation Products ◽  
Internal Standard ◽  
Dosage Forms ◽  
Uv Detector ◽  
Stability Indicating ◽  
Therapeutic Benefits ◽  
Relative Standard

Background: Axitinib (AXT) is a member of the new generation of the kinase inhibitor indicated for the treatment of advanced renal cell carcinoma. Its therapeutic benefits depend on assuring the good-quality of its dosage forms in terms of content and stability of the pharmaceutically active ingredient. Objective: This study was devoted to the development of a simple, sensitive and accurate stabilityindicating high-performance liquid chromatographic method with ultraviolet detection (HPLC-UV) for the determination of AXT in its bulk and dosage forms. Methods: Waters HPLC system was used. The chromatographic separation of AXT, internal standard (olaparib), and degradation products were performed on the Nucleosil CN column (250 × 4.6 mm, 5 μm). The mobile phase consisted of water:acetonitrile:methanol (40:40:20, v/v/v) with a flow rate of 1 ml/min, and the UV detector was set at 225 nm. AXT was subjected to different accelerated stress conditions and the degradation products, when any, were completely resolved from the intact AXT. Results: The method was linear (r = 0.9998) in the concentration range of 5-50 μg/ml. The limits of detection and quantitation were 0.85 and 2.57 μg/ml, respectively. The accuracy of the method, measured as recovery, was in the range of 98.0-103.6% with relative standard deviations in the range of 0.06-3.43%. The results of stability testing revealed that AXT was mostly stable in neutral and oxidative conditions; however, it was unstable in alkaline and acidic conditions. The kinetics of degradation were studied, and the kinetic rate constants were determined. The proposed method was successfully applied for the determination of AXT in bulk drug and dosage forms. Conclusions: A stability-indicating HPLC-UV method was developed and validated for assessing AXT stability in its bulk and dosage forms. The method met the regulatory requirements of the International Conference on Harmonization (ICH) and the Food and Drug Administration (FDA). The results demonstrated that the method would have great value when applied in quality control and stability studies for AXT.

scholarly journals Validated stability indicating methods for determination of nitazoxanide in presence of its degradation products

2012 ◽  
Vol 2 (2) ◽  
pp. 105-116 ◽  
Author(s):  
Nouruddin W. Ali ◽  
Samah Sayed Abbas ◽  
Hala El-Sayed Zaazaa ◽  
Maha Mohamed Abdelrahman ◽  
Mohamed Abdelkawy
Keyword(s):  
Degradation Products ◽  
Stability Indicating
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