Bioanalytical method development and validation for the determination of glycine in human cerebrospinal fluid by ion-pair reversed-phase liquid chromatography–tandem mass spectrometry

2016 ◽  
Vol 128 ◽  
pp. 132-140 ◽  
Author(s):  
Jian Jiang ◽  
Christopher A. James ◽  
Philip Wong
Keyword(s):  
Method Development ◽  
Reversed Phase ◽  
Reversed Phase Liquid Chromatography ◽  
Chromatography Tandem Mass Spectrometry ◽  
Human Cerebrospinal Fluid ◽  
Liquid Chromatography Tandem Mass ◽  
Method Development And Validation ◽  
Phase Liquid ◽  
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.

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