Method development and validation of selective and highly sensitive method for determination of apixaban in human plasma using liquid chromatography-tandem mass spectrometry
By: Atmakuri, Chaitanya Krishna
.
Contributor(s): Prasad, Cheepurupalli.
Publisher: Bhopal Innovare Academic Sciences Pvt Ltd 2019Edition: Vol. 11(8).Description: 39-45p.Subject(s): PHARMACEUTICSOnline resources: Click here
In:
International journal of pharmacy and pharmaceutical scienceSummary: 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.
Keywords: Human Plasma, Liquid Chromatography-Tandem, Mass
| Item type | Current location | Call number | Status | Date due | Barcode | Item holds |
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Articles Abstract Database
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School of Pharmacy Archieval Section | Not for loan | 2020021 |
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.
Keywords: Human Plasma, Liquid Chromatography-Tandem, Mass
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