scholarly journals Characterization of novel stress degradation products of Bempedoic acid and Ezetimibe using UPLC–MS/MS: development and validation of stability-indicating UPLC method

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Anuradha Vejendla ◽  
Subrahmanyam Talari ◽  
G. Ramu ◽  
Ch Rajani
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Orthophosphoric Acid ◽  
Degradation Products ◽  
Chemical Structures ◽  
Stress Studies ◽  
Stress Degradation ◽  
Development And Validation ◽  
Simultaneous Assessment

Abstract Background A receptive and easily comprehended technique was evolved for simultaneous assessment of Bempedoic acid and Ezetimibe and its impurities characterized by UPLC–MS/MS. Results This technique involves chromatographic separation with a C18 column of water symmetry (150 mm × 4.6 mm, 3.5 µm). A mobile phase of 0.1% OPA (orthophosphoric acid) and acetonitrile in 50:50 v/v with 1 mL/min flow rate and ambient temperature was used. UV observation was taken at 230 nm. The recoveries, linearity, and quantification limits were found to be within the acceptable limit. Conclusions This technique was successfully tested with UPLC–MS to confirm the chemical structures of newly formed degradation products of Bempedoic acid and Ezetimibe and stress studies as per ICH Q2 (R1) guidelines.

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.

Stability-Indicating Determination of Tedizolid Phosphate in the Presence of its Active Form and Possible Degradants

2021 ◽  
Author(s):  
Eman M Moaaz ◽  
Ezzat M Abdel-Moety ◽  
Mamdouh R Rezk ◽  
Ahmed S Fayed
Keyword(s):  
Flow Rate ◽  
Phosphate Buffer ◽  
Mobile Phase ◽  
Degradation Products ◽  
Active Form ◽  
Pharmaceutical Formulations ◽  
Bacterial Strains ◽  
Stress Degradation ◽  
Tlc Plates

Abstract Tedizolid phosphate is an antibiotic prodrug that is metabolized into tedizolid which is used against various resistant bacterial strains. In this study, tedizolid phosphate was subjected to stress degradation conditions, namely, hydrolysis (neutral, acidic and alkaline), thermal, oxidative and photolytic ones. The prodrug was stable toward thermal and photolytic stress conditions, while it showed significant degradation upon applying oxidative and hydrolytic conditions. Two suggested chromatographic methods are described for separation and determination of tedizolid phosphate from the resulted degradation products. The first method is HPLC using Waters Xselect HSS C18 (250 × 4.6 mm, 5 μm) analytical column and mobile phase composed of phosphate buffer (50 mM, pH 6.5):acetonitrile (70:30, %v/v) pumped at flow rate of 1.0 mL/min with UV-detection at 300 nm. The second method is a TLC coupled with densitometric quantitation, precoated silica TLC-plates as a stationary phase and a mobile phase of methanol:butanol:ethyl acetate:ammonia (33%, w/v) (60:20:20:10,%v/v) were used. The chromatographed plates were scanned at 300 nm. The linearity was confirmed over concentration range of 1–100 μg/mL and 1–12 μg/band for HPLC and TLC-densitometric methods, respectively. Both methods were found to be suitable for determination of tedizolid phosphate in pure form and in its pharmaceutical formulations.

scholarly journals LC-MS characterization of acid degradation products of metoclopramide: Development and validation of a stability-indicating RP-HPLC method

2020 ◽  
Vol 11 (1) ◽  
pp. 781-789
Author(s):  
Sriram Valavala ◽  
Nareshvarma Seelam ◽  
Subbaiah Tondepu ◽  
Suresh Kandagatla
Keyword(s):  
Liquid Chromatography ◽  
Mobile Phase ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Hplc Technique

The present study aims to develop a simple, accurate and specific stability-indicating RP-HPLC technique for the analysis of metoclopramide in the presence of its stress degradation products and characterization of degradation compounds by LC-MS/MS analysis. As per ICH Q1A-R2 guidelines, the drug was exposed to acid hydrolytic stress condition. Three degradation products were formed for MCP in acid hydrolysis. The liquid chromatography was processed on a Luna C18-(2) 100A,250×4.6mm 5micron column using an isocratic mobile phase consisting of 0.1% formic acid in water-acetonitrile (20:80, v/v) by adjusting the mobile phase at 1 ml/min flow rate with wavelength detection at 273 nm. The developed procedure was applied to LC-MS/MS (liquid chromatography-tandem mass spectrometry) for the characterization of all the degradant components. Total new three degradation compounds were recognized and identified by LC-MS/MS. The developed RP-HPLC technique was validated as per the ICH Q2-R1 guidelines. Limit of detection and limit of quantification values of MCP were evaluated from the linearity graph and were found to be 5.23 µg/ml and 17.44 µg/ml. Accuracy study was established at 80.0, 100.0 and 120.0 µg/ml concentration levels and the findings were found in the range of 98.4% - 101.8%. The linearity of the technique was assessed over the drug concentration range of 50.0 µg/ml to 250.0 µg/ml and the regression equation, slope and correlation coefficient values were found to be y = 10618x + 1623.2, 10618 and 0.9996 respectively. The developed technique was uninterruptedly applied for the quantification of metoclopramide inactive pharmaceuticals.

Identification and structural characterization of the stress degradation products of omeprazole using Q-TOF-LC-ESI-MS/MS and NMR experiments: evaluation of the toxicity of the degradation products

2019 ◽  
Vol 43 (19) ◽  
pp. 7294-7306 ◽  
Author(s):  
G. Shankar ◽  
Roshan M. Borkar ◽  
Suresh Udutha ◽  
M. Kanakaraju ◽  
G. Sai Charan ◽  
...  
Keyword(s):  
Gastroesophageal Reflux Disease ◽  
Proton Pump Inhibitor ◽  
Gastroesophageal Reflux ◽  
Degradation Products ◽  
Forced Degradation ◽  
Peptic Ulcers ◽  
Ich Guidelines ◽  
Stress Degradation ◽  
Forced Degradation Studies

Omeprazole (OMP), a prototype proton pump inhibitor used for the treatment of peptic ulcers and gastroesophageal reflux disease (GERD), was subjected to forced degradation studies as per ICH guidelines Q1A (R2).

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