Research article Received: 28 July 2014,

Revised: 13 December 2014,

Accepted: 31 December 2014

Published online in Wiley Online Library: 2 February 2015

(wileyonlinelibrary.com) DOI 10.1002/bmc.3435

Quantification of polygalasaponin F in rat plasma using liquid chromatography–tandem mass spectrometry and its pharmacokinetics application Wenli Zhoua, Jiantao Zhangb, Wei Xua and Jinghui Suna* ABSTRACT: A rapid and highly selective liquid chromatography–tandem mass spectrometric (LC-MS/MS) method for determination of polygalasaponin F (PF) in rat plasma was developed and validated. The chromatographic separation was achieved on a reverse-phase Zorbax SB-C18 column (150 × 4.6 mm, 5 μm), using 2 mM ammonium acetate (pH adjusted to 6.0 with acetic acid) and acetonitrile (25:75, v/v) as a mobile phase at 30 °C. MS/MS detection was performed using an electrospray ionization operating in positive ion multiple reaction monitoring mode by monitoring the ion transitions from m/z 1091.5 → 471.2 (PF) and m/z 700.4 → 235.4 (internal standard), respectively. The calibration curve showed a good linearity in the concentration range 0.0544–13.6 μg/mL, with a limit of quantification of 0.0544 μg/mL. The intra- and inter-day precisions were 0.9950. The representative regression equation for the calibration curves during validation was y = 7.1914 × 10 7x + 2.6683 × 10 5, r = 0.9969. The LOQ value for the analyte was 54.4 ng/mL, which was sufficient for pharmacokinetic studies of PF after intravenous administration of three different dosages in rats with a signal-to-noise ratio (S/N)>10.

20000

16000

Precision (RSD %)

12000 10000 8000

Accuracy and precision

6000

Intra- and inter-day data for accuracy and precision in plasma are presented in Table 1. All of the obtained values were well within with the published guidelines (US DHHS et al., 2013). Intra- and inter-day variations were established by analyzing the samples (n = 6) at three QC concentrations of 136, 1360 and 12,240 ng/mL on three separate days. The precision (relative standard deviation, RSD) calculated by QC samples was

Quantification of polygalasaponin F in rat plasma using liquid chromatography-tandem mass spectrometry and its pharmacokinetics application.

A rapid and highly selective liquid chromatography-tandem mass spectrometric (LC-MS/MS) method for determination of polygalasaponin F (PF) in rat plas...
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