Development and validation of LC‐QTOF‐MS/MS method for identification and determination of low levels of a genotoxic impurity, 4,6‐dichloro‐5‐nitro‐2‐(propylthio) pyrimidine in ticagrelor API

2022 ◽  
Author(s):  
Manchuri Krishna Moorthy ◽  
Shaik Mahammad Ali ◽  
Gopireddy Venkata Subba Reddy
Keyword(s):  
Low Levels ◽  
Development And Validation

scholarly journals Development and Validation of Confirmatory Method for Analysis of Nitrofuran Metabolites in Milk, Honey, Poultry Meat and Fish by Liquid Chromatography-Mass Spectrometry

2016 ◽  
Vol 39 (1) ◽  
pp. 15-22 ◽  
Author(s):  
Fatih Alkan ◽  
Arzu Kotan ◽  
Nurullah Ozdemir
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Solid Phase ◽  
Poultry Meat ◽  
Fish Samples ◽  
Low Levels ◽  
Reported Data ◽  
Development And Validation ◽  
Nitrofuran Metabolites

AbstractIn this study we have devoloped and validated a confirmatory analysis method for nitrofuran metabolites, which is in accordance with European Commission Decision 2002/657/EC requirements. Nitrofuran metabolites in honey, milk, poultry meat and fish samples were acidic hydrolised followed by derivatisation with nitrobenzaldehyde and liquid-liquid extracted with ethylacetate. The quantitative and confirmative determination of nitrofuran metbolites was performed by liquid chromatography/electrospray ionisation tandem mass spectrometry (LC/ESI-MS/MS) in the positive ion mode. In-house method validation was performed and reported data of validation (specificity, linearity, recovery, CCα and CCβ). The advantage of this method is that it avoids the use of clean-up by Solid-Phase Extraction (SPE). Furthermore, low levels of nitrofuran metabolites are detectable and quantitatively confirmed at a rapid rate in all samples.

Development and Validation of Derivative Spectroscopic Method for Simultaneous Estimation of Cefadroxil and Probenecid

2014 ◽  
Vol 7 (1) ◽  
pp. 2350-2355
Author(s):  
Pratik S Mehta ◽  
Pratik R. Patel ◽  
Rajesh R Parmar ◽  
M M K Modasiya ◽  
Dushyant A Shah
Keyword(s):  
Spectroscopic Method ◽  
Spectral Interference ◽  
Synthetic Mixture ◽  
Simultaneous Estimation ◽  
Zero Crossing ◽  
First Order ◽  
Derivative Spectroscopy ◽  
Development And Validation ◽  
Crossing Point

A novel, simple, accurate, sensitive, precise and economical derivative spectroscopic method was developed and validated for the determination of cefadroxil and probenecid in synthetic mixture. First order derivative spectroscopy method was adopted to eliminate spectral interference. The method obeys Beer’s Law in concentration ranges of 4-36 μg/ml for cefadroxil and of 5-25 μg/ml of probenecid. The zero crossing point for cefadroxil and probenecid was 260 nm and 237.8 nm respectively in 0.1N HCl. The method was validated in terms of accuracy, precision, linearity, limits of detection, limits of quantitation. This method has been successively applied to synthetic mixture and no interference from the synthetic mixture’s excipients was found.   

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