Norisoboldine (NIB) is one of the main bioactive isoquinoline alkaloids in Linderae Radix. A rapid, selective and sensitive method using UPLC-ESI/MS was first developed for simultaneous determination of NIB and norisoboldine-9-O-alpha-glucuronide (NIB-Glu), its major metabolite in rat plasma. A one-step protein precipitation with methanol was employed as sample preparation technique. Chromatographic separation was carried out on an Acquity UPLC BEH C(18) column (50 x 2.1 mm, i.d. 1.7 mu m) with a gradient mobile phase consisting of acetonitrile and water containing 0.1% formic acid. Detection and quantification were performed using a quadrupole mass spectrometer by selective ion reaction-monitoring mode. Good linearity was achieved using weighted (1/x(2)) least squares linear regression over the concentration ranges 0.01-2 mu g/mL for NIB and 0.025-25 mu g/mL for NIB-Glu. The lower limit of quantification of NIB and NIB-Glu was 0.01 and 0.025 mu g/mL, respectively. The intra-and inter-day precisions (relative standard deviations) of the assay at all three quality control levels were 4.6-14.1% for NIB, and 5.0-12.2% for NIB-Glu. The accuracies (relative error) were -13.5-8.1% for NIB and -12.8-7.6% for NIB-Glu, respectively. This developed method was successfully applied to an in vivo pharmacokinetic study in rats after a single intravenous dose of 10 mg/kg NIB. Copyright (C) 2010 John Wiley & Sons, Ltd.
[1]Shanghai Univ Tradit Chinese Med, MOE Key Lab Standardizat Chinese Med, Inst Chinese Mat Med, Shanghai 201203, Peoples R China.
[2]Shanghai Univ Tradit Chinese Med, SATCM Key Lab New Resources & Qual Evaluat Chines, Inst Chinese Mat Med, Shanghai 201203, Peoples R China.
[3]China Pharmaceut Univ, Dept Pharmacognosy, Nanjing 210038, Peoples R China.
[4]Shanghai R&D Ctr Standardizat Chinese Med, Shanghai 201203, Peoples R China.
(8.0+极速模式)