Determination of the concentration of β-D-glucopyranosyl-3-(O-β-D-glucopyranosyl-oxy)-oleanolate in rat plasma by ultra performance liquid chromatography and tandem mass spectrometry
10.13699/j.cnki.1001-6821.2018.03.039
- VernacularTitle:超高效液相色谱串联质谱快速测定大鼠血浆的鸡骨草皂苷含量
- Author:
Ming CAO
1
;
Yun-Fang ZHOU
;
Wen-Tian XIE
Author Information
1. 天台县人民医院药剂科
- Keywords:
Achyranthes aspera L saponin;
UPLC-MS/MS;
pharmacokinetics;
plasma concentration
- From:
The Chinese Journal of Clinical Pharmacology
2018;34(3):319-322
- CountryChina
- Language:Chinese
-
Abstract:
Objective To determine the concentration ofβ-D-gluco-pyranosy1-3-(0-β-D-glucopyranosyloxy)-oleanolate (AA-2) in rat plasma by ultra performance liquid chromatography and tandem mass spectrometry (UPLC-MS/MS) method.Methods Plasmas were separated from the heparinized whole blood by centrifugation.After addition of chlorzoxazone as an internal standard (IS),protein precipitation by acetonitrile-methanol (9∶1) was used to prepare samples.Chromatographic separation was achieved on a UPLC BEH C18column (2.1 mm × 100 mm,1.7 μm) with 0.1％ formic acid and acetonitrile as the mobile phase with gradient elution.An electrospray ionization source was applied and operated in negative ion mode.Multiple reactions monitoring (MRM) mode was used for quantification using target fragment ions m/z 793.5→631.4 for AA-2,and m/z 168.1→132.1 for IS.Results Calibration plots were linear throughout the range of 10-5000 ng · mL-1 for AA-2 in rat plasma.Mean recoveries of AA-2 in rat plasma ranged from 70.4％ to 87.8％.RSD of intra-day and inter-day precision were both less than 10％.The accuracy of the method was between 91.1％ and 104.1％.After intravenous administration of AA-2(1,3,5 mg · kg-1),the mean residence time(MRT0-t) were (0.32 ±0.13),(0.48 ±0.15),(0.44±0.08) h.The i1/2 were (1.15±0.72),(1.32 ± 0.90),(1.02 ± 0.22) h.The CL were (4.53±1.66),(4.44 ±0.94),(4.86±0.49) L · h-1 · kg-1 The Cmax were (681.67 ±246.78),(1809.45 ±479.11),(4953.21 ± 722.72) ng· mL-1.Conclusion The method was simple,rapid and sensitive,which was suitable for pharmacokinetics study of AA-2 after intravenous administration in rats.
