scholarly journals Isolation, Identification and Characterization of Gefitinib Novel Degradation Products by NMR and HRMS, Method Development and Validation by UPLC

2021 ◽  
Vol 33 (8) ◽  
pp. 1743-1748
Author(s):  
Ramulu Yanaka ◽  
Hima Bindu Gandham ◽  
Chidananda Swamy Rumalla ◽  
Muralidharan Kaliyaperumal ◽  
Shaik John Saida ◽  
...  
Keyword(s):  
Method Development ◽  
Degradation Products ◽  
2D Nmr ◽  
The Novel ◽  
Ich Guidelines ◽  
Stress Degradation ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Identification And Characterization

Gefitinib (GFT) sold under the brand name Iressa, is a medication used to treat certain type of breast, lung and other cancers, Gefitinib was subject to stress degradation under acidic, basic, peroxide mediated oxidation, photolytic and thermal degradation. The stress degradation was performed according to ICH guidelines Q1A(R2) and the drug was inert under thermal and photolytic conditions. One degradant is identified in acid hydrolysis referred as 7-methoxy-6-(3-morpholinopropoxy) quinazolin-4(3H)-one (GFT-DP1) and two degradants were formed in peroxide mediated hydrolysis referred as 4-(3-((4-((3- chloro-4-fluorophenyl)amino)-7-methoxy-1-oxidoquinazolin-6-yl)oxy)-propyl)morpholine-4-oxide (GFT-DP2) and 4-(3-((4-((3-chloro-4-fluorophenyl)amino)-7-methoxyquinazolin-6-yl)oxy)-propyl)- morpholine-4-oxide (GFT-DP3). In present study, all the novel three degradation product structures were confirmed by HRMS and 1D (1H, 13C) and 2D (COSY, HSQC and HMBC) based on 1D and 2D NMR data proton and carbon chemical shift values assigned exactly for all degradation products. A stability indicating RP-UPLC method was developed and validated with shorter run time and this method was validated in terms of linearity, specificity, accuracy, LOD and LOQ.

scholarly journals Identification and Characterization of Two New Forced Degradation Products of Saikosaponin a under the Stress of Acid Hydrolytic Condition

2016 ◽  
Author(s):  
Jun Li ◽  
Qiang Xu ◽  
Hua Jiang
Keyword(s):  
Method Development ◽  
Degradation Products ◽  
Forced Degradation ◽  
Worst Case ◽  
Method Performance ◽  
Stability Indicating Method ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Saikosaponin A

Saikosaponin (SS) a is a compound with various pharmacological properties and easily degraded into SSb1 and SSg in acid condition. In present work another two new degradation products of SSa formed under acid hydrolytic condition were detected and isolated by analytical and semi-preparative liquid chromatography technology, furthermore their structures were characterized as hydroxyl-saikosaponin a and SSb2 by spectral analysis, which is not only essential in stability-indicating method development and validation but also could be used as a worst case to assess the analytical method performance of SSa. Moreover their structural transformation pathways were also proposed.

High Performance HPLC-UV Method Development and Validation for Sulfadoxine from its Potential Interfering Impurities

2021 ◽  
Vol 08 ◽  
Author(s):  
Nayan S. Gadhari ◽  
Jayram V. Gholave ◽  
Suyog S. Patil ◽  
Ajay R. Patil ◽  
Kiran F. Shelke ◽  
...  
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Method Development ◽  
Degradation Products ◽  
Drug Product ◽  
Ich Guidelines ◽  
Daunting Task ◽  
Method Development And Validation ◽  
The Stability ◽  
Development And Validation

Objective: To address the separation of interfering potential impurities associated with the drug is always a daunting task. We present the method validation and quantitative determination of sulfadoxine (SUL), an anti-malarial drug with most important interfering impurities present pharmaceutical dosages and in bulk samples using HPLC-UV method. Methods: The UV detection was obtained at 270 nm and SUL is separated on Sunfire C18 (25 cm x 4.6 mm x 5 µ m) column at 45°C with flow rate of 1.0 mL/min in a mobile phase (CH3COOH:CH3CN). The stress testing (acidic/basic/oxidative) was performed using HPLC for SUL and its impurities showing the highly efficient separation peaks between degradant and drug product. Results: The developed method was found to be highly accurate and sensitive in regulation with ICH guidelines. Also, it was found to be free from interference from degradation products which allows the stability indicating capability of developed HPLC-UV method for SUL for validation in bulk drugs. Conclusion: The main advantages of the present method; (a) Separation achieved in 30 minutes, (b) MS compatible mobile phase renders this developed method can be directly adapted to LC-MS without any major modifications in near future, and (c) separation of twelve impurities on Sunfire C18 column. The CFs (correction factors) had been calculated for all the impurities. It was found to be 1.6 (IMP IX), 1.70 (IMP XI) and in between 0.8-1.3 for all other impurities. The LOD of the developed method for all the analytes were in the range of 0.05 to 0.11 μg/mL and the LOQ values were in the range of 0.17 to 0.36 μg/mL.

scholarly journals Stability indicating method development and validation for simultaneous estimation and quantification of Ertugliflozin and Metformin in bulk and tablet dosage form

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Bhawani Sunkara ◽  
Tulja Rani Gampa ◽  
Mounika Markanti ◽  
Ratna Kumari Midthapally
Keyword(s):  
Method Development ◽  
Degradation Products ◽  
Simultaneous Estimation ◽  
Elution Time ◽  
Stability Indicating Method ◽  
Ich Guidelines ◽  
Simultaneous Evaluation ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Tablet Dosage

Abstract Background A simple, economical, sensitive, authentic, and faithful technique was used for the study of simultaneous evaluation of Ertugliflozin and Metformin in tablet dosage forms. The Chromatographic analysis was performed isocratically by using a Phenomenex C18 column (150 mm × 4.6 mm, 5 μm), and a mobile phase containing acetonitrile and 0.1% OPA buffer, with a proportion of 40: 60% v/v was passed throughout the column maintained at a temperature of 30 °C with a flow rate of 1 ml/min. Approximately, 10 μl of drug solution was injected and the analytes were eluted at 220.0 nm. Results The elution times of Ertugliflozin and Metformin were 2.226 min and 2.955 min, respectively. The percentage RSD of Ertugliflozin and Metformin are 0.60 and 0.59, respectively. The percentage recoveries of Ertugliflozin and Metformin were determined to be 100.55% and 99.40%, respectively. LOD, LOQ values of Metformin and Ertugliflozin obtained were found to be 0.10, 0.2 μg/ml and 0.03, 0.09 μg/ml, respectively. Regression equation of Ertugliflozin was y = 11287x + 1191 and y = 46270x + 161.0 for Metformin. All verification parameters are within the range according to the ICH guidelines, and the degradation products are also within the limits, which show that the method is stable. Conclusion In the currently developed RP-HPLC analytical method, the elution time and run time is reduced, which proves that the method is economical and widely acceptable, also simple and practical, which can be used in routine quality control tests in the industry.

scholarly journals RP-HPLC method development and validation for estimation of rivaroxaban in pharmaceutical dosage forms

2013 ◽  
Vol 49 (2) ◽  
pp. 359-366 ◽  
Author(s):  
Mustafa Çelebier ◽  
Tuba Reçber ◽  
Engin Koçak ◽  
Sacide Altinöz
Keyword(s):  
Method Development ◽  
Internal Standard ◽  
Hplc Method ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Method Development And Validation ◽  
Hplc Method Development ◽  
Development And Validation ◽  
Tablet Dosage

Rivaroxaban, an anti-clotting medication, acts at a crucial point in the blood-clotting process and stops the formation of blood clots. In this study, RP-HPLC method was developed for the determination of rivaroxaban in tablets (Xarelto® (10 mg)). Phenomenex Luna 5 µm C18 100 Å LC Column (250 x 4.6 mm) was used at 40 ºC. Isocratic elution was performed with ACN:Water (55:45 v/v) mixture. The flow rate was 1.2 mL min-1 and UV detection was at 249 nm. Internal standard (Caffeine) and rivaroxaban were eluted within 2.21 and 3.37 minutes, respectively. The developed method was validated according to the ICH guidelines and found to be linear within the range 0.005 - 40.0 µg mL-1. The method was accurate, precise, robust and rapid. Thus, it was applied successfully for the quality control assay of rivaroxaban in tablet dosage form.

LC–UV method development and validation for the investigational anticancer agent imexon and identification of its degradation products

2005 ◽  
Vol 38 (4) ◽  
pp. 686-694 ◽  
Author(s):  
Monique W.J. den Brok ◽  
Bastiaan Nuijen ◽  
Michel J.X. Hillebrand ◽  
Christian Lutz ◽  
Hans-Georg Opitz ◽  
...  
Keyword(s):  
Method Development ◽  
Anticancer Agent ◽  
Degradation Products ◽  
Method Development And Validation ◽  
Development And Validation

Analytical Method Development and Validation of Glipizide to Determine Residual solvents by head Space-Gas Chromatography

2021 ◽  
pp. 2440-2444
Author(s):  
Sanapala Srinivasa Rao ◽  
A. Vijayalakshmi
Keyword(s):  
Gas Chromatography ◽  
Method Development ◽  
Limit Of Detection ◽  
Dimethyl Formamide ◽  
Analytical Methodology ◽  
Residual Solvents ◽  
Flame Ionization ◽  
Ich Guidelines ◽  
Method Development And Validation ◽  
Development And Validation

Residual solvents in Pharmaceuticals are termed as organic volatile impurities. These are the chemicals that are used in the manufacture of drug substance or excipients or use in the preparation of final formulation. Most of the available methods use liquid chromatography which could be expensive and time consuming. Hence, an analytical methodology was developed for the quantification of residual solvents in Glipizide using a headspace gas chromatography (HSGC) with the help of flame ionization detector (FID). Methanol, acetone and dimethyl formamide as residual solvents were determined in Glipizide. Analysis was performed by headspace GC/FID method on Auto system- HS40. Nitrogen was used as a carrier gas and the separation of residual solvents was achieved by DB-Wax 0.25mm, 0.3mcm column. The thermostat temperature was 115 °C for 40 minutes for each vial. % RSD for nine injections obtained are in acceptance criteria. The correlation coefficient R2 obtained greater than 0.99. The method parameters were validated includes specificity, limit of detection and quantification, accuracy, linearity, precision, and robustness. According to the International Conference on Harmonization (ICH) guidelines, a new simple, specific, accurate and precise method was developed and validated.

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