scholarly journals Method development and validation of Guanfacine in rat plasma by liquid chromatography–tandem mass spectrometry: Application to a pharmacokinetic study

2013 ◽  
Vol 3 (6) ◽  
pp. 472-480
Author(s):  
Suryanarayana Murthy Goparaju ◽  
Yadagiri Srinivasa Murthy Nandula ◽  
Chandrasekher Bannoth Kothapalli ◽  
B.R. Challa ◽  
Bahlul Z. Awen
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Method Development ◽  
Rat Plasma ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Mass Spectrometry Application

scholarly journals METHOD DEVELOPMENT AND VALIDATION STUDY FOR QUANTITATIVE DETERMINATION OF GENOTOXIC IMPURITY AND ITS PRECURSOR IN FLUCONAZOLE SAMPLE BY LIQUID CHROMATOGRAPHY–TANDEM MASS SPECTROMETRY

2016 ◽  
Vol 8 (12) ◽  
pp. 84
Author(s):  
L. Narasimha Rao K ◽  
N. Devanna ◽  
K.v.n. Suresh Reddy
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Method Development ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass ◽  
Method Development And Validation ◽  
Development And Validation

<p><strong>Objective: </strong>The objective of this work is method development and validation study for quantitative determination of 1-[2-(2,4-difluorophenyl)-2,3-epoxypropyl]-1H-1,2,4-triazole, a genotoxic impurity and its precursor in a fluconazole drug sample by liquid chromatography–tandem mass spectrometry.</p><p><strong>Methods: </strong>LC-MS/MS analysis of these impurities was performed on Hypersil BDS C18 (100 mm x 4.0 mm, 3 µm) column. 5 mmol ammonium acetate and acetonitrile in the ratio of 65:35 (v/v) was used as the mobile phase with a flow rate of 0.4 ml/min. The developed method was accomplished with a short run time of 10 min. Triple quadrupole mass detector coupled with positive electrospray ionization was used for the quantification of genotoxic impurities in multiple reaction monitoring (MRM).</p><p><strong>Results: </strong>The method was validated as per International Conference on Harmonization (ICH) guidelines. The method was linear in the range of 0.30 µg/g to 11.37 µg/g for impurity A and 0.30 µg/g to 11.34 µg/g for impurity B with a correlation coefficient of 0.999. The accuracy of the method was in the range of 98.25 % to 100.53 % for both impurities.</p><p><strong>Conclusion: </strong>A specific, selective, highly sensitive and more accurate analytical method using LC-MS/MS coupled with positive electrospray ionization has been developed for the quantification of genotoxic impurity (1-[2-(2,4-difluorophenyl)-2,3-epoxypropyl]-1H-1,2,4-triazole) and its precursor (1-(2,4-difluorophenyl)-2-[1,2,4]triazol-1-yl-ethanone) at 0.3 µg/g with respect to the 5.0 mg/ml of fluconazole.</p>

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