Τίτλος:
Determination of nateglinide in human plasma by high-performance liquid chromatography with pre-column derivatization using a coumarin-type fluorescent reagent
Γλώσσες Τεκμηρίου:
Αγγλικά
Περίληψη:
A sensitive and selective high-performance liquid chromatographic method has been developed and validated for the determination of nateglinide in human plasma. Nateglinide and the internal standard, undecylenic acid, were extracted from plasma by liquid-liquid extraction using a mixture of ethyl acetate-diethyl ether, 50:50 (v/v). Pre-column derivatization reaction was performed using a coumarin-type fluorescent reagent, N-(7-methoxy-4-methyl-2-oxo-2H-6-chromenyl)-2-bromoacetamide. The derivatization proceeded in acetone in the presence of potassium carbonate and catalyzed by 18-crown-6 ether. The fluorescent derivatives were separated under isocratic conditions on a Hypersil BDS-C8 analytical column (250.0 mm × 2.1 mm i.d., particle size 5 μm) with a mobile phase that consisted of 65% acetonitrile in water and pumped at a flow rate of 0.50 mL min-1. The excitation and emission wavelengths were set at 345 and 435 nm, respectively. The assay was linear over a concentration range of 0.05-16.00 μg mL-1 for nateglinide with a limit of quantitation of 0.05 μg mL-1. Quality control samples (0.05, 4.50 and 16.00 μg mL-1) in five replicates from five different runs of analysis demonstrated intra-assay precision (%coefficient of variation <6.8%), inter-assay precision (%coefficient of variation <1.6%) and an overall accuracy (%relative error) less than -3.4%. The method can be used to quantify nateglinide in human plasma covering a variety of pharmacokinetic or bioequivalence studies. © 2007 Elsevier B.V. All rights reserved.
Συγγραφείς:
Malli, D.
Gikas, E.
Vavagiannis, A.
Kazanis, M.
Daniilides, K.
Gennimata, D.
Panderi, I.
Περιοδικό:
Analytica Chimica Acta
Λέξεις-κλειδιά:
Fluorescent reagents; Nateglinide; Pre-column fluorescence derivatization; Undecylenic acid, Extraction; High performance liquid chromatography; Particle size; Pharmacokinetics; Plasma (human); Potash; Wavelength, Drug products, 10 undecenoic acid; acetic acid ethyl ester; acetone; acetonitrile; acetylsalicylic acid; candesartan hexetil; coumarin; ether; lepur; n (7 methoxy 4 methyl 2 oxo 2h 6 chromenyl) 2 bromoacetamide; nateglinide; omeprazole; penrazol; potassium carbonate; propafenone; reagent; salospir; simvastatin; unclassified drug; water, accuracy; adult; article; catalysis; derivatization; drug blood level; drug determination; drug structure; field emission; flow rate; fluorescence analysis; high performance liquid chromatography; human; human experiment; liquid liquid extraction; male; particle size; priority journal; quality control, Acetamides; Chromatography, High Pressure Liquid; Coumarins; Cyclohexanes; Fluorescent Dyes; Humans; Hypoglycemic Agents; Indicators and Reagents; Phenylalanine; Reproducibility of Results
DOI:
10.1016/j.aca.2007.08.004
