Rapid and sensitive UPLC-MS/MS method for the determination of etodolac in small-volume rat plasma: Application to rat real samples

A rapid, simple, and sensitive UPLC-MS/MS method was developed and validated for the determination of etodolac in rat plasma using flurbiprofen as an internal standard (IS). Etodolac and IS were detected using electrospray ionization in negative ion multiple reaction monitoring mode by monitoring th...

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Bibliographic Details
Published in:Journal of liquid chromatography & related technologies 2018-05, Vol.41 (9), p.474-480
Main Authors: Yaman, Mehmet Emrah, Kocak, Omer Faruk, Atila, Alptug, Kadioglu, Yucel, Diyarbakir, Busra, Halici, Zekai
Format: Article
Language:English
Subjects:
Ammonium
Bioanalytical method validation
Calibration
Chromatography
etodolac
Flow velocity
Flurbiprofen
Ionization
Ions
Linearity
liquid phase extraction
Monitoring
Negative ions
Plasma
rat plasma
Solvents
tandem mass spectrometry
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Summary:A rapid, simple, and sensitive UPLC-MS/MS method was developed and validated for the determination of etodolac in rat plasma using flurbiprofen as an internal standard (IS). Etodolac and IS were detected using electrospray ionization in negative ion multiple reaction monitoring mode by monitoring the transitions (precursor to product) m/z 286.2→212.1 and 243.2→199.2, respectively. The developed new extraction procedure for etodolac in rat plasma does not contain more than one stage. Chromatographic separation was performed on reverse phase C 18 column with a gradient mobile phase, which consisted of methanol for solvent A and 5 mM ammonium formate in water solvent B percentages varying at a flow rate of 0.4 mL/min. The LLOQ for etodolac was determined as 1 ng/mL. The calibration curve for etodolac was linear (r > 0.996 for plasma) well within the range of 1-5000 ng/mL. Quantification of etodolac in rat plasma is possible in a short chromatographic run time (1.91 min) with this method. The proposed method was fully validated by determining specificity, linearity, LLOQ, precision and accuracy, recovery, matrix effect, and stability. The validated method was successfully applied to plasma samples obtained from rats.
ISSN:1082-6076
1520-572X
DOI:10.1080/10826076.2018.1464474