scholarly journals Determination of ceftriaxone in human plasma using liquid chromatography–tandem mass spectrometry

2019 ◽  
Vol 4 ◽  
pp. 47 ◽  
Author(s):  
Thamrong Wongchang ◽  
Markus Winterberg ◽  
Joel Tarning ◽  
Natthida Sriboonvorakul ◽  
Sant Muangnoicharoen ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Human Plasma ◽  
Matrix Effects ◽  
Internal Standard ◽  
Selected Reaction Monitoring ◽  
Pharmacokinetic Studies ◽  
Tandem Mass ◽  
Antibiotic Drug

Ceftriaxone is a cephalosporin antibiotic drug used as first-line treatment for several bacterial diseases. Ceftriaxone belongs to the third generation of antibiotics and is available as an intramuscular or intravenous injection. Previously published pharmacokinetic studies have mainly used high-performance liquid chromatography coupled with ultraviolet detection (HPLC-UV) for the quantification of ceftriaxone. This study aimed to develop and validate a bioanalytical method for the quantification of ceftriaxone in human plasma using liquid chromatography followed by tandem mass spectrometry (LC-MS/MS). Sample preparation was performed by protein precipitation in combination with phospholipid-removal techniques for cleaning up matrix interferences. The chromatographic separation was performed on an Agilent Zorbax Eclipse Plus C18 column with 10 mM ammonium formate containing 2% formic acid: acetonitrile as mobile phase at a flow rate of 0.4 ml/min. Both the analyte and cefotaxime (internal standard) were quantified using the positive electrospray ionization (ESI) mode and selected reaction monitoring (SRM) for the precursor-product ion transitions m/z 555.0→396.1 for ceftriaxone and 456.0→324.0 for cefotaxime. The method was validated over the concentration range of 1.01-200 μg/ml. Calibration response showed good linearity (correlation coefficient > 0.99) and no significant matrix effects were observed. The intra-assay and inter-assay precision were less than 5% and 10%, respectively, and therefore well within standard regulatory acceptance criterion of ±15%.

scholarly journals Determination of ceftriaxone in human plasma using liquid chromatography–tandem mass spectrometry

2021 ◽  
Vol 4 ◽  
pp. 47
Author(s):  
Thamrong Wongchang ◽  
Markus Winterberg ◽  
Joel Tarning ◽  
Natthida Sriboonvorakul ◽  
Sant Muangnoicharoen ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Human Plasma ◽  
Internal Standard ◽  
Selected Reaction Monitoring ◽  
Tandem Mass ◽  
Antibiotic Drug ◽  
Citrate Phosphate Dextrose ◽  
Citrate Phosphate

Ceftriaxone is a cephalosporin antibiotic drug used as first-line treatment for a number of bacterial diseases. Ceftriaxone belongs to the third generation of antibiotics and is available as an intramuscular or intravenous injection. Previously published pharmacokinetic studies have used high-performance liquid chromatography coupled with ultraviolet detection (HPLC-UV) for the quantification of ceftriaxone. This study aimed to develop and validate a bioanalytical method for the quantification of ceftriaxone in human plasma using liquid chromatography followed by tandem mass spectrometry (LC-MS/MS). Sample preparation was performed by protein precipitation of 100 µl plasma sample in combination with phospholipid-removal techniques to minimize matrix interferences. The chromatographic separation was performed on an Agilent Zorbax Eclipse Plus C18 column with 10 mM ammonium formate containing 2% formic acid: acetonitrile as mobile phase at a flow rate of 0.4 ml/min with a total run time of 10 minutes. Both the analyte and cefotaxime (internal standard) were quantified using the positive electrospray ionization (ESI) mode and selected reaction monitoring (SRM) for the precursor-product ion transitions m/z 555.0→396.1 for ceftriaxone and 456.0→324.0 for cefotaxime. The method was validated over the concentration range of 1.01-200 μg/ml. Calibration response showed good linearity (correlation coefficient > 0.99) and matrix effects were within the ±15% limit in 6 different lots of sodium heparin plasma tested. However, citrate phosphate dextrose plasma resulted in a clear matrix enhancement of 24% at the low concentration level, which was not compensated for by the internal standard. Different anticoagulants (EDTA, heparin and citrate phosphate dextrose) also showed differences in recovery. Thus, it is important to use the same anticoagulant in calibration curves and clinical samples for analysis. The intra-assay and inter-assay precision were less than 5% and 10%, respectively, and therefore well within standard regulatory acceptance criterion of ±15%.

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.

scholarly journals DEVELOPMENT AND VALIDATION OF LIQUID CHROMATOGRAPHY COUPLED WITH TANDEM MASS SPECTROMETRY METHOD FOR ESTIMATION OF LENVATINIB IN HUMAN PLASMA

2017 ◽  
Vol 10 (7) ◽  
pp. 120
Author(s):  
Srikanth I ◽  
Prameela Rani A
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Human Plasma ◽  
Internal Standard ◽  
Correlation Coefficients ◽  
Tandem Mass ◽  
Liquid Chromatography Tandem Mass ◽  
Positive Mode ◽  
Development And Validation

Objective: This study was to develop and validate a liquid chromatography–tandem mass spectrometry (LC–MS/MS) for the quantification of lenvatinib (LT) in human plasma.Methods: A simple, sensitive and specific LC–MS/MS method was developed for quantification of LT in human plasma using LTD4 as internal standard (IS). The analytical method consists of liquid–liquid extraction of plasma sample followed by the determination of LT by a LC–MS/MS. The analyte was separated on a Zorbax Eclipse XDB-C18 (150×4.6 mm, 5 μ) column with an isocratic mobile phase of acetontrile:0.1% formic acid (80:20 v/v) at a flow rate of 0.6 mL/minutes. The protonated ions were formed by a turbolon spray in a positive mode were used to detect analyte and IS. The MS/MS detection was made by monitoring the fragmentation of m/z 427.10→370.10 for LT and m/z 430.30→370.10 for IS on a MS.Result: The method was validated with the correlation coefficients of (r2) ≥0.995 over a linear concentration range of 10.20-501.60 pg/mL. This method demonstrated intra- and inter-day precision within 1.06-2.42% and 0.03-0.55% and accuracy within 95.64-100.08% and 97.16-100.07%.Conclusion: This method is suitable and convenient to pharmacokinetics and bioavailability studies for estimation of LT in biological samples by LC–MS/MS.

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.

Development and validation of bioanalytical liquid chromatography–tandem mass spectrometry method for the estimation of pentoxifylline in human plasma: Application for a comparative pharmacokinetic study

2018 ◽  
Vol 25 (4) ◽  
pp. 372-380 ◽  
Author(s):  
Sireesha Dodda ◽  
Ajitha Makula ◽  
Srinivasa R Polagani ◽  
Raj N Kandhagatla
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Human Plasma ◽  
Pharmacokinetic Study ◽  
Internal Standard ◽  
Tandem Mass ◽  
Comparative Pharmacokinetic ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

A method for bioanalysis of pentoxifylline in human plasma was developed using liquid chromatography–tandem mass spectrometry, which is simple, specific, and sensitive. Pentoxifylline D5 was used as the internal standard. Employing only 100 µl of human plasma, processing was done with solid-phase extraction technique. The analyte and the internal standard were separated from endogenous components on Ace phenyl column using a mixture of 5 mM ammonium acetate buffer and high performance liquid chromatography grade acetonitrile (60:40, v/v) as mobile phase at a flow rate of 1 ml/min. The linearity of the method was in the range of 3–1200 ng/ml with r2 > 0.99. Positive ion MRM mode was used for the detection of the analyte and the internal standard. The method was validated as per the US Food and Drug Administration guidelines and the results were within the acceptance limits. The proposed method was applied for comparative pharmacokinetic study of pentoxifylline after oral administration of 400 and 600 mg tablets to South Indian male subjects under fed conditions.

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