RESUMEN
Objective: To study the chemical constituents in acid hydrolysates of Panax notoginseng saponins (PNS). Methods: These compounds were separated and purified by column chromatography, and their structures were elucidated based on spectroscopic analyses (HR-ESI-MS, ESI-MS, 1H-NMR, 13C-NMR, HSQC and HMBC). Results: Eighteen compounds were obtained from the acid hydrolysates of PNS and characterized as dammar-25-ene-24-hydroperoxyl-3β,6α,12β,20S-tetraol (1), 6α,12β,20S-trihydroxy- dammarane-24-ene-3-O-β-D-glucopyranosyl-(1→2)-β-D-glucopyranoside (2), 6α,12β,20R-trihydroxy-dammarane-24-ene-3-O-β-D- glucopyranosyl-(1→2)-β-D-glucopyranoside (3), vina-ginsenoside-R8 (4), 24(S)-pseudo-ginsenoside-GQ (5), ginsenoside Rg5 (6), 20 (R)-ginsenoside Rg3 (7), 20(R)-ginsenoside Rk2 (8), 3β,12β-dihydroxy-dammar-(E)-20(22),24-diene-6-O-β-D-xylopyranosyl- (1→2)-β-D-glucopyranoside (9), 20(S)-ginsenoside Rg2 (10), ginsenoside SL1 (11), 20(R)-ginsenoside Rh1 (12), 20(22) E-ginsenoside Rh4 (13), 25-hydroxy-20(R) ginsenoside-Rh1 (14),3β,6α,12β,20(S)-20,25-epoxy-3,12-dihydroxy-dammarane-6-O-β-D-glucopyranoside (15), 20(R)-protopanaxadiol (16), 20(R)-protopanaxatriol (17), and 20(S)-protopanaxatriol (18). Conclusion: Compound 1 is a new triterpen saponin, and compounds 2-5 are isolated from P. notoginseng and acid dydrolysates of PNS for the first time.
RESUMEN
Objective To evaluate the uncertainty of the pseudo-ginsenoside GQ (PGQ) concentration in human plasma by HPLC-MS/MS.Methods The whole process of PGQ determination by HPLC-MS/MS in human plasma was evaluated and the uncertainty caused by repeatability,weighing,standard solution preparation,biological sample preparation,extraction recovery process,recovery,instrument precision and calibration curve fitting were evaluated,respectively.The combined and expanded uncertainty values were both calculated.Results The expanded uncertainty values for low (15.16 ng·mL-1),medium (2 516.67 ng·mL-1) and high (3 902.00 ng·mL-1) levels of PGQ were 1.39,177.74 and 262.69 ng·mL-1,respectively (P =95 ％,k =2).Conclusion The uncertainty of the PGQ determination in human plasma by HPLC-MS/MS is mainly caused by recovery,repeatabihty and sample preparation at low concentration,by sample preparation and recovery at medium and high concentration.