scholarly journals Determination of Apixaban Levels in Human Plasma by a High-Throughput Liquid Chromatographic Tandem Mass Spectrometry Assay / Determinarea rapidă a apixabanului în plasma umană prin cromatografie de lichide de înaltă performanță cuplată cu spectrometrie de masă în tandem

2015 ◽  
Vol 23 (1) ◽  
Author(s):  
Ioan Țilea ◽  
Daniela Saveta Popa ◽  
Timea Szakács Xantus ◽  
Daniela Primejdie ◽  
Bianca Grigorescu ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Tandem Mass Spectrometry ◽  
Human Plasma ◽  
High Throughput ◽  
Multiple Reaction Monitoring ◽  
Therapeutic Drug ◽  
Pharmacokinetic Studies ◽  
Tandem Mass ◽  
Rapid Preparation ◽  
Chromatography Method

AbstractA high-throughput liquid chromatography method with detection by tandem mass spectrometry (LC-MS/MS) was developed and validated for the quantification of apixaban in human plasma. The separation was performed on a Gemini-NX column under isocratic conditions using a 33:67 (v/v) mixture of acetonitrile and 1 mM ammonium formate in water at 40 ºC with a flow rate of 0.5 mL/min. The detection of apixaban was performed in multiple reaction monitoring mode (m/z 417.2 from m/z 460.2) with electrospray positive ionization. A single-step protein precipitation with methanol was used for plasma sample preparation. The method was validated with respect to selectivity, linearity (r > 0.994), intra-day and inter-day precision (CV < 14.4 %) and accuracy (bias < 9.5 %) over the range of 9.70 - 970.00 ng/mL plasma. The lower limit of quantification (LLOQ) was 9.70 ng/mL and the recovery was between 97.4 - 104.5 %. The method is fast, efficient, requires the processing of a small volume of plasma (50 μL), a short run-time (1 min) for chromatographic analysis, and a simple and rapid preparation of samples. It is very well suited for clinical therapeutic drug monitoring and pharmacokinetic studies.

A Novel Simultaneous Estimation of Sofosbuvir and Velpatasvir in Human Plasma by Liquid Chromatography Tandem-Mass Spectrometry after Protein Precipitation Method

2019 ◽  
Vol 15 (7) ◽  
pp. 710-715
Author(s):  
S.T. Narenderan ◽  
Basuvan Babu ◽  
T. Gokul ◽  
Subramania Nainar Meyyanathan
Keyword(s):  
Mass Spectrometry ◽  
Tandem Mass Spectrometry ◽  
Human Plasma ◽  
Multiple Reaction Monitoring ◽  
Simultaneous Estimation ◽  
Pharmacokinetic Studies ◽  
Tandem Mass ◽  
Mass Spectrometric Method ◽  
Highly Sensitive ◽  
Tandem Mass Spectrometric

Objective: The aim of the present work is to achieve a novel highly sensitive chromatographic method for the simultaneous determination of hepatitis C agents, sofosbuvir and velpatasvir from human plasma using ritonavir as an internal standard. Methods: Chromatographic separation was achieved using Hypersil C18 column (50mm x 4.6mm, 3μm) with an isocratic elution mode using the mobile phase composition 10 mM ammonium formate buffer (pH 5.0): acetonitrile (20:80 v/v) pumped at a flow rate of 0.5 ml/min. The detection was carried out by tandem mass spectrometry using Multiple Reaction Monitoring (MRM) positive Electrospray Ionization (ESI) with proton adducts at m/z 530.10 > 243.10, 883.40 > 114.0 and 721.25 > 197.0. Results: The method validated as per USFDA guidelines with respect to linearity, accuracy, and precision was found to be acceptable over the concentration range of 0.2–2000 ng/ml and 5-2000 ng/ml for sofosbuvir and velpatasvir respectively and the method was found to be highly sensitive and selective. Conclusion: The developed tandem mass spectrometric method is robust and can be applied for the monitoring of plasma levels of the analyzed drug in preclinical and clinical pharmacokinetic studies.

scholarly journals Quantification and Validation of Ertapenem Using a Liquid Chromatography-Tandem Mass Spectrometry Method

2014 ◽  
Vol 58 (6) ◽  
pp. 3481-3484 ◽  
Author(s):  
S. P. van Rijn ◽  
A. M. A. Wessels ◽  
B. Greijdanus ◽  
D. J. Touw ◽  
J. W. C. Alffenaar
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Human Plasma ◽  
Internal Standard ◽  
Therapeutic Drug ◽  
Pharmacokinetic Studies ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

ABSTRACTErtapenem, a carbapenem, relies on time-dependent killing. Therapeutic drug monitoring (TDM) should be considered, when ertapenem is used in specific populations, to achieve optimal bactericidal activity and optimize drug-dosing regimens. No validated liquid chromatography-tandem mass spectrometry (LC-MS/MS) method has been reported using deuterated ertapenem as the internal standard. A new simple and robust LC-MS/MS method using a quadrupole mass spectrometer was developed for analysis of ertapenem in human plasma, using deuterated ertapenem as the internal standard. The calibration curve was linear over a range of 0.1 (lower limit of quantification [LLOQ]) to 125 mg/liter. The calculated accuracy ranged from −2.4% to 10.3%. Within-run coefficients of variation (CV) ranged from 2.7% to 11.8%, and between-run CV ranged from 0% to 8.4%. Freeze-thaw stability had a bias of −3.3% and 0.1%. Storage of QC samples for 96 h at 4°C had a bias of −4.3 to 5.6%, storage at room temperature for 24 h had a bias of −10.7% to −14.8%, and storage in the autosampler had a bias between −2.9% and −10.0%. A simple LC-MS/MS method to quantify ertapenem in human plasma using deuterated ertapenem as the internal standard has been validated. This method can be used in pharmacokinetic studies and in clinical studies by performing TDM.

Development of Sensitive and High-Throughput Liquid Chromatography–Tandem Mass Spectrometry Method for Quantification of Haloperidol in Human Plasma with Phospholipid Removal Pretreatment

2020 ◽  
Author(s):  
Nela Zidekova ◽  
Adam Nemcek ◽  
Martina Sutovska ◽  
Juraj Mokry ◽  
Martin Kertys
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Therapeutic Drug Monitoring ◽  
Tandem Mass Spectrometry ◽  
Human Plasma ◽  
Therapeutic Drug ◽  
Tandem Mass ◽  
Extraction Recovery ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

Abstract Haloperidol, butyrophenone derivative, is a typical antipsychotic drug used in the treatment of schizophrenia, manic phase of bipolar disorder, and acute psychomotor agitations. According to the recent guidelines for therapeutic drug monitoring, it is strongly recommended to measure plasma level during the therapy with haloperidol. The objective of this study was to develop and validate a simple liquid chromatography–tandem mass spectrometry-based method to quantitate haloperidol in human plasma. After one-step extraction procedure using OSTROTM plate, gradient elution on Acquity UPLC BEH C18 (50 × 2.1 mm, 1.7 μm) column over 3.2 min was performed. The detection was conducted on a triple quadrupole tandem mass spectrometer by multiple reaction monitoring mode in positive ionization mode with transitions at m/z 376.29 → 165.14 and m/z 380.28 → 169.17 for haloperidol and haloperidol-d4 (used as an internal standard), respectively. The method was fully validated to cover wide concentration range of 0.05–80 ng/mL in human plasma and meets the criteria for the selectivity, linearity and lower limit of detection, precision and accuracy, matrix effect, extraction recovery, carryover, dilution integrity and stability. The extraction recovery was nearly 100%, and no significant matrix effects were observed. Therefore, the method is applicable to routine therapeutic drug monitoring in patients’ plasma.

scholarly journals A Hydrophilic Interaction Liquid Chromatography–Tandem Mass Spectrometry Quantitative Method for Determination of Baricitinib in Plasma, and Its Application in a Pharmacokinetic Study in Rats

Molecules ◽  
2020 ◽  
Vol 25 (7) ◽  
pp. 1600 ◽  
Author(s):  
Essam Ezzeldin ◽  
Muzaffar Iqbal ◽  
Yousif A. Asiri ◽  
Azza A Ali ◽  
Prawez Alam ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Janus Kinase ◽  
Pharmacokinetic Studies ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

Baricitinib, is a selective and reversible Janus kinase inhibitor, is commonly used to treat adult patients with moderately to severely active rheumatoid arthritis (RA). A fast, reproducible and sensitive method of liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the quantification of baricitinib in rat plasma has been developed. Irbersartan was used as the internal standard (IS). Baracitinib and IS were extracted from plasma by liquid–liquid extraction using a mixture of n-hexane and dichloromethane (1:1) as extracting agent. Chromatographic separation was performed using Acquity UPLC HILIC BEH 1.7 µm 2.1 × 50 mm column with the mobile phase consisting of 0.1% formic acid in acetonitrile and 20 mM ammonium acetate (pH 3) (97:3). The electrospray ionization in the positive-mode was used for sample ionization in the multiple reaction monitoring mode. Baricitinib and the IS were quantified using precursor-to-production transitions of m/z 372.15 > 251.24 and 429.69 > 207.35 for baricitinib and IS, respectively. The method was validated according to the recent FDA and EMA guidelines for bioanalytical method validation. The lower limit of quantification was 0.2 ng/mL, whereas the intra-day and inter-day accuracies of quality control (QCs) samples were ranged between 85.31% to 89.97% and 87.50% to 88.33%, respectively. Linearity, recovery, precision, and stability parameters were found to be within the acceptable range. The method was applied successfully applied in pilot pharmacokinetic studies.

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