Development and Validation of an HPLC Method for Quantification of Filgotinib, a Novel JAK-1 Inhibitor in Mice Plasma: Application to a Pharmacokinetic Study

Drug Res (Stuttg) DOI: 10.1055/a-1141-3475Filgotinib is a selective JAK1 (Janus kinase) inhibitor, filed in Japan for
the treatment of rheumatoid arthritis. In this paper, we present the data of
development and validation of a high-performance liquid chromatography
(HPLC) method for the quantitation of filgotinib in mice plasma as per the
FDA regulatory guideline. The method involves the extraction of filgotinib
along with internal standard (IS, tofacitinib) from mice plasma
(100 µL) using ethyl acetate as an extraction solvent. The
chromatographic analysis was performed using an isocratic mobile phase
comprising 10 mM ammonium acetate (pH 4.5) and acetonitrile (70:30,
v/v) at a flow-rate of 0.8 mL/min on a Hypersil Gold
C18 column. The UV detection wavelength was set at
λmax 300 nm. Filgotinib and the IS eluted at 5.56 and
4.28 min, respectively with a total run time of 10 min. The
calibration curve was linear over a concentration range of 0.05 to
5.00 μg/mL (r
2+=≥0.992). The intra- and inter-day
precision and accuracy results were within the acceptable limits. Results of
stability studies indicated that filgotinib was stable on bench-top, in
auto-sampler, up to three freeze/thaw cycles and long-term storage
at −80°C. The valida...

Source: Drug Research - April 13, 2020 Category: Drugs & Pharmacology Authors: Zakkula, Ashok Pulipati, Shobha Dittakavi, Sreekanth Bestha, Ram Murthi Zainuddin, Mohd Trivedi, Ravi Kumar Mullangi, Ramesh Tags: Original Article Source Type: research