title: Comparison of LC-UV and LC-MS methods for simultaneous determination of teriflunomide, dimethyl fumarate and fampridine in human plasma: application to rat pharmacokinetic study.
abstract: This study describes a comparison between LC-UV and LC-MS method for the simultaneous analyses of a few disease-modifying agents of multiple sclerosis. Quantitative determination of fampridine (FAM), teriflunomide (TFM) and dimethyl fumarate (DMF) was performed in human plasma with the recovery values in the range of 85-115%. A reversed-phase high-performance liquid chromatography (HPLC) with UV as well as MS detection is used. The method utilizes an XBridge C18 silica column and a gradient elution with mobile phase consisting of ammonium formate and acetonitrile at a flow rate of 0.5 mL min(-1) . The method adequately resolves FAM, TFM and DMF within a run time of 15 min. Owing to low molecular weights, the estimation of DMF and FAM is more versatile in UV than MS detection. With LC-UV, the detection limits of FAM, TFM and DMF were 0.1, 0.05, 0.05 μg and the quantification limit for all the analytes was 1 μg. With LC-MS, the detection and quantification limits for all of the analytes were 1 and 5 ng, respectively. The two techniques were completely validated and shown to be reproducible and sensitive. They were applied to a pharmacokinetic study in rats by a single oral dose. Copyright © 2016 John Wiley & Sons, Ltd.
authors: Department of Pharmaceutical Analysis, Hindu College of Pharmacy, Amaravathi road, Guntur, -522 002, Andhra Pradesh, India.
authors: A
authors: A
authors: Suneetha
authors: College of Pharmaceutical Sciences, Acharya Nagarjuna University, Nagarjuna Nagar, Guntur, -522510, Andhra Pradesh, India.
authors: Rajeswari K
authors: RK
authors: Raja
mesh_terms: D015761:4-Aminopyridine / Q000097:blood* / Q000493:pharmacokinetics; D000818:Animals; D002853:Chromatography, Liquid / Q000379:methods*; D003437:Crotonates / Q000097:blood* / Q000493:pharmacokinetics; D000069462:Dimethyl Fumarate / Q000097:blood* / Q000493:pharmacokinetics; D006801:Humans; D006885:Hydroxybutyrates; D013058:Mass Spectrometry / Q000379:methods*; D009570:Nitriles; D051381:Rats; D012015:Reference Standards; D015203:Reproducibility of Results; D013056:Spectrophotometry, Ultraviolet / Q000379:methods*; D014052:Toluidines / Q000097:blood* / Q000493:pharmacokinetics
chemical_list: D003437:Crotonates; D006885:Hydroxybutyrates; D009570:Nitriles; D014052:Toluidines; C527525:teriflunomide; D015761:4-Aminopyridine; D000069462:Dimethyl Fumarate
keywords: LC-UV and LC-MS; dimethyl fumarate; fampridine; multiple sclerosis; pharmacokinetics; teriflunomide