| Autor: |
Mogili, Ramakotaiah, Kanala, Kanchanamala, Challa, Balasekhara, Chandu, Babu, Bannoth, Chandrasekhar |
| Zdroj: |
Chromatographia; Oct2011, Vol. 74 Issue 7/8, p585-592, 8p |
| Abstrakt: |
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 (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. 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 with correlation coefficient r ≥ 0.9981. The limit of quantification (LOQ) and limit of detection (LOD) were found to be 0.1 ng mL 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. [ABSTRACT FROM AUTHOR] |
| Databáze: |
Complementary Index |
| Externí odkaz: |
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