title: Simultaneous determination of atorvastatin and niacin in human plasma by LC-MS/MS and its application to a human pharmacokinetic study.
abstract: A rapid, simple, sensitive and selective LC-MS/MS method has been developed and validated for quantification of the atorvastatin (AT) and niacin (NA) in 250 μL human plasma. The analytical procedure involves a liquid-liquid extraction method using nevirapine as an internal standard (IS). The chromatographic separation was achieved on a Hypurity Advance (4.6 × 50 mm, 5 µm) column using a mobile phase consisting of 0.1% formic acid buffer-acetonitrile (20:80, v/v) at flow rate of 0.8 mL/min. The API-4000 LC-MS/MS was operated in the multiple-reaction monitoring mode using electrospray ionization. The total run time of analysis was 3 min and elution of AT, NA and IS occurred at 1.06, 1.84 and 0.92 min, respectively. A detailed validation of the method was performed as per the US Food and Drug Administration guidelines and the standard curves found to be linear in the range of 0.10-30.0 ng/mL for AT and 20.2-6026 ng/mL for NA, with a coefficient of correlation of ≥ 0.99 for both the compounds. AT and NA were found to be stable in a battery of stability studies, viz. bench-top, autosampler, re-injection, wet-extract and repeated freeze-thaw cycles. The developed assay method was successfully applied to a pharmacokinetic study in humans.
authors.affiliation: Research Studies, Rayalaseema University, Kurnool-518 002, India.
authors.forename: Vasu Babu
authors.initials: VB
authors.lastname: Ravi
authors.forename: Ramesh
authors.initials: R
authors.lastname: Mullangi
authors.forename: Jaswanth Kumar
authors.initials: JK
authors.lastname: Inamadugu
authors.forename: Nageswara Rao
authors.initials: NR
authors.lastname: Pilli
authors.forename: Ramakrishna
authors.initials: R
authors.lastname: Gajula
authors.forename: Venkateswarlu
authors.initials: V
authors.lastname: Ponneri
mesh_terms: D000069059:Atorvastatin; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004355:Drug Stability; D006538:Heptanoic Acids / Q000097:blood* / Q000737:chemistry / Q000493:pharmacokinetics; D006801:Humans; D016014:Linear Models; D059625:Liquid-Liquid Extraction; D008297:Male; D019829:Nevirapine / Q000097:blood; D009525:Niacin / Q000097:blood* / Q000737:chemistry / Q000493:pharmacokinetics; D011758:Pyrroles / Q000097:blood* / Q000737:chemistry / Q000493:pharmacokinetics; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D006538:Heptanoic Acids; D011758:Pyrroles; D009525:Niacin; D019829:Nevirapine; D000069059:Atorvastatin