A method coupling ultra-performance liquid chromatography (UPLC) with quadrupole time-of-flight mass spectrometer (Qtof MS) using the electrospray ionization (ESI) source was developed for the identification of the major saponins from Panax notoginseng powder (PNP). Ten different PNP samples were analyzed and evaluated for their quality by similarity evaluation and principle component analysis (PCA). Based on the accurate mass, summarized characteristic fragmentation behaviors, retention times of different types of saponins, related botanical biogenesis, and reported chromatographic behavior of saponins, fifty-one common peaks were effectively separated and identified, including 28 protopanaxadiol saponins and 18 protopanaxatriol saponins. Simultaneously, 15 significant discrepancy compounds were identified from the disqualified PNP samples. The established UPLC/Qtof MS fingerprint method was successfully applied for profiling and identifying the major saponins of PNP, providing a fast quality evaluation tool for distinguishing the authentic PNP and the adulterated products.
Chromatography, High Pressure Liquid ; methods ; Drugs, Chinese Herbal ; chemistry ; Panax notoginseng ; chemistry ; Powders ; chemistry ; Spectrometry, Mass, Electrospray Ionization ; methods

Objective: To investigate the stamina,the role of antioxidant system in severe acute pancreatitis(SAP),and the effect of fish oil treatment in rats.Methods:Thirty-six male Sprague-Dawley rats(SD) were randomly divided into three groups,including SAP group(sodium chloride treatment ) (group NSG,n=12),fish oil treatment group (group FOG,n=12),and control group (group CG,n=12).SAP was induced by intergraded injection of 3.5% sodium tanrocholate to biliopancreatic duct of SD rats in group NSG and FOG.The group NSG rats were treated by subcutaneous injection of sodium chloride,while the group FOG rats were treated by subcutaneous injection of fish oil for 7 days.Then the improved tail suspension test was observed at the first,third,fifth,seventh day.12 rats in each group were respectively sacrificed after 7 day.The activity of serum antioxidant enzymes (MDA,GSH-PH) and the concentration of serum amylase were measured in each group,and the levels of threshold on the area and the total immobility time were measured in each group.The severity of pancreatitis was analyzed according to the histopathological morphology.Results: Compared to group NSG,the severity of pancreatitis was significantly decreased in group FOG.The activity of MDA was significantly increased in group NSG than that in group CG (P<0.01) ,while the activity of MDA in group FOG was decreased than that in group NSG (P<0.05) .The activity of GSH-PH was significantly decreased in group NSG than that in group CG(P<0.01),while the activity of GSH-PH was increased in group GOG than that in group NSG (P<0.05).THE level of threshold on the area was decreased in group NSG than that in group CG(P<0.01),while the level of threshold on the area was increased in group GOG than that in group NSG.(P<0.01) The total immobility time was significantly increased in group NSG than that in group CG(P<0.01),while the total immobility time was decreased in group GOG than that in group NSG(P<0.05).MDA was associated with the level of threshold on the area and the total immobility time.Conclusion: Fish oil has a positive effect on the activity of antioxidant system and behavior character in SAP rats.

PURPOSE: A simple, rapid, and highly sensitive analytical method for Gb3 in plasma was developed without labor-extensive pre-treatment by electrospray ionization MS/MS (ESI-MS/MS). Measurement of globotriaosylceramide (Gb3, ceramide trihexoside) in plasma has clinical importance for monitoring after enzyme replacement therapy in Fabry disease patients. The disease is an X-linked lipid storage disorder that results from a deficiency of the enzyme ??-galactosidase A (alpha-Gal A). The lack of alpha-Gal A causes an intracellular accumulation of glycosphingolipids, mainly Gb3. METHODS: Only simple 50-fold dilution of plasma is necessary for the extraction and isolation of Gb3 in plasma. Gb3 in diluted plasma was dissolved in dioxane containing C17:0 Gb3 as an internal standard. After centrifugation it was directly injected and analyzed through guard column by in combination with multiple reaction monitoring mode of ESI-MS/MS. RESULTS: Eight isoforms of Gb3 were completely resolved from plasma matrix. C16:0 Gb3 occupied 50% of total Gb3 as a major component in plasma. Linear relationship for Gb3 isoforms was found in the range of 0.001-1.0 microgram/mL. The limit of detection (S/N=3) was 0.001 microgram/mL and limit of quantification was 0.01 microgram/mL for C16:0 Gb3 with acceptable precision and accuracy. Correlation coefficient of calibration curves for 8 Gb3 isoforms ranged from 0.9678 to 0.9982. CONCLUSION: This quantitative method developed could be useful for rapid and sensitive 1st line Fabry disease screening, monitoring and/or diagnostic tool for Fabry disease.