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摘要
A rapid and sensitive liquid chromatography-tandem mass spectrometric (LC-MS/MS) method for the simultaneous quantitation of five major active ingredients of Ixeris sonchifolia (Bge.) Hance in rat plasma has been developed and validated. After liquid-liquid extraction of 50 mu L plasma with ethyl acetate, analytes and internal standard (I.S.), astilbin, were chromatographed on a Zorbax SB-C18 column (150 mm x 4.6 mm, 5 mu m) using acetonitrile - 10 mM ammonium acetate (60:40, v/v, pH 5.6) as mobile phase. The five analytes: chicoric acid, luteolin 7-O-beta-D-glucuronide, luteolin 7-O-beta-D-glucopyranoside, luteolin 7-O-beta-D-glucopyranosyl-(1 --> 2)-beta-D-glucopyranoside, apigenin 7-O-beta-D-glucuronide and I.S., were detected by negative ion electrospray ionization followed by multiple reaction monitoring of the ions with m/z 473.0 --> 311.0, 461.0 --> 285.0, 447.0 --> 285.0, 609.1 --> 285.0, 445.1 --> 269.0 and 449.1 --> 150.9, respectively. The method was linear for all analytes in the concentration range 10-3000 ng/mL with intra- and inter-day precision (as relative standard deviation) <= 8.99% and accuracy (as relative error) <= 4.00%. The limits of detection (LOD) were 5, 1, 5, 5,2 ng/mL for chicoric acid, luteolin 7-O-beta-D-glucuronide, luteolin 7-O-beta-D-glucopyranoside, luteolin 7-O-beta-D-glucopyranosyl-(1 --> 2)-beta-D-glucopyranoside, apigenin 7-O-beta-D-glucuronide, respectively. The method was successfully applied to a pharmacokinetic study of the five analytes in rat after a single intravenous dose of Kudiezi Injection.
- 出版日期2013-7-15
- 单位吉林大学
