Method development and validation for quantitative determination of methadone enantiomers in human plasma by liquid chromatography/tandem mass spectrometry1

2004 ◽  
Vol 806 (2) ◽  
pp. 191-198 ◽  
Author(s):  
H LIANG ◽  
R FOLTZ ◽  
M MENG ◽  
P BENNETT
Keyword(s):  
Liquid Chromatography ◽  
Quantitative Determination ◽  
Human Plasma ◽  
Method Development ◽  
Tandem Mass ◽  
Liquid Chromatography Tandem Mass ◽  
Method Development And Validation ◽  
Development And Validation

scholarly journals METHOD DEVELOPMENT AND VALIDATION OF SELECTIVE AND HIGHLY SENSITIVE METHOD FOR DETERMINATION OF APIXABAN IN HUMAN PLASMA USING LIQUID CHROMATOGRAPHY-TANDEM MASS SPECTROMETRY

2019 ◽  
pp. 39-45
Author(s):  
CHAITANYA KRISHNA ATMAKURI ◽  
CHEEPURUPALLI PRASAD ◽  
RAJARAM S. PATIL ◽  
KARUNAKRANTH DHARANI
Keyword(s):  
Human Plasma ◽  
Method Development ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Highly Sensitive ◽  
Liquid Chromatography Tandem Mass ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Sensitive Method

Objective: The present research work aims to develop and validate a selective and highly sensitive method for the determination of apixaban in human plasma using liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods: 200 µl of sodium heparin plasma samples were acidified and clean-up was performed by using solid-phase extraction (SPE). Apixaban 13C D3 was used as an internal standard (deuterated) to lower the relative matrix effects and a single step SPE was employed for sample clean up. 10 µl of SPE eluent was loaded onto Hypersil Beta Basic C18, 100×4.6 mm, 5 µ column for highly selective chromatographic separation using an isocratic mobile phase. 2 mmol ammonium acetate in water and acetonitrile were delivered by using a quaternary low-pressure gradient pump without premixing at a minimum flow rate of 0.50 ml/min. Results: LC-MS/MS method was successfully developed and validated to demonstrate the lowest detection limit of 0.05 ng/ml and a linear dynamic range from 1-250 ng/ml with r2>0.99. Method development and validation results proved that the method is selective and highly sensitive for the determination of apixaban in human plasma using LC-MS/MS. Conclusion: Current method can be applied for both therapeutic drug monitoring (TDM) and pharmacokinetic (PK) study analysis.

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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