Determination of Rizatriptan in Human Plasma by Liquid Chromatography Stable Isotope Dilution Electrospray MS–MS for Application in Bioequivalence Study

Autor: Ramakotaiah Mogili, Kanchanamala Kanala, Chandrasekhar Kothapalli Bannoth, Babu R. Chandu, Balasekhara R. Challa
Rok vydání: 2011
Předmět:
Zdroj: Chromatographia. 74:585-592
ISSN: 1612-1112
0009-5893
DOI: 10.1007/s10337-011-2110-7
Popis: A simple, sensitive, selective, rapid, rugged, reproducible and specific liquid chromatography–tandem mass spectrometry (LC–MS/MS) method was used for quantitative estimation of rizatriptan (RZ) in human plasma using rizatriptan-d 6 (RZD6) as internal standard (IS). Chromatographic separation was performed on Ascentis Express RP Amide C18, 50 × 4.6 mm, 2.7 μm column with isocratic mobile phase composed of 10 mM ammonium formate:acetonitrile (20:80 v/v) at flow rate of 0.5 mL min−1. RZ and RZD6 were detected with proton adducts at m/z (amu) 270.2 → 201.2 and 276.1 → 207.1, respectively, in multiple reaction monitoring (MRM) positive mode. Liquid–liquid extraction was used and validated over a linear concentration range of 0.1–100.0 ng mL−1 with correlation coefficient r 2 ≥ 0.9981. The limit of quantification (LOQ) and limit of detection (LOD) were found to be 0.1 ng mL−1 and 12.5 fg, respectively. Intra- and inter-day precision were within 1.7–3.1% and 2.8–3.7%, and accuracy within 96.0–101.7% and 99.7–101.4% for RZ. Drug was found to be stable throughout three freeze–thaw cycles. The method was successfully employed for analysis of plasma samples following oral administration of RZ (10 mg) in 25 healthy Indian male human volunteers under fasting conditions.
Databáze: OpenAIRE
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