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A method for qualitative analysis of constituents in Panax notoginseng by UPLC-LTQ-Orbitrap mass spectrometry was established. Based on the high-resolution mass information, MS/MS fragmentation behaviors and chemical components from literatures, 43 compounds were identified or tentatively characterized. New type saponin aglycone, combined with malonyl-substituted and acetyl-substituted saponins were discovered and plausibly identified in this study. This work could be helpful for the quality control and further phytochemical studies of Panax notoginseng, and provided a good example for the analysis of chemical constituents in traditional Chinese medicine.
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Five compounds, huyouyisu (1), vomifoliol (2), isoferulic acid (3), 1,2,3-trihydroxy-phenol (4) and p-hydroxy-phenol (5), were isolated from the peels of Citrus changshan-huyou Y.B.Chang for the first time by utilizing repeated column chromatography on silica gel. Among them, huyouyisu (1) is a new compound. The structure was elucidated by using 1D and 2D spectra.
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A new compound and twelve known compounds were isolated from the ethyl acetate extract of the roots of Homonoia riparia Lour, which are used in folk medicine for treatment of hepatitis, bellyache and scald, by the method of silica gel column chromatography repeatedly with a gradient of PE-EtOAc, PE-Me2CO, CHCl3-Me2CO, CHCl3-MeOH. Their structures were identified as a new compound 1-oxo-aleuritolic acid (1), and twelve known compounds aleuritolic acid (2), 3-acetoxy-aleuritolic acid (3), taraxerone (4), taraxerol (5), methyl 3-acetoxy-12-oleanen-28-oate (6), 3-acetoxy-12-oleanen-28-ol (7), ursolic acid (8), lupenol (9), 3β-acetoxy-lupenol (10), cleomiscosin A (11), chrysophanol (12), and gallic acid (13), which were obtained from this plant for the first time, by the spectroscopic techniques of NMR, HMBC, IR and MS, separately. Among the cytotoxicities evaluation of compounds 1-3 towards AGZY 83-a (human lung cancer cells) and SMMC-7721 (human liver cancer cells) tumor cells was assayed by MTT methods with cis-dichlorodiamminoplatinum (DDP) used as positive control. Compound 2 exerted weak activity against AGZY 83-a with the IC50 value of 33.055 μg·mL-1, while 1 and 3 showed no activity to these two cell lines.
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OBJECTIVE: To study the therapeutic mechanism of salvianolic acid B (SA-B) in treating hepatic fibrosis. METHODS: Twenty-four Wistar rats were randomly divided into 3 groups: normal control group, untreated group and SA-B-treated group. Rats in the untreated and SA-B-treated groups were injected intraperitoneally with 0.5% dimethylnitrosamine (DMN) for 4 weeks, daily for 3 days each week at a dose of 10 microg/kg, to induce hepatic fibrosis. Then, rats in the SA-B-treated group were given SA-B orally for another 4 weeks. Hydroxyproline (Hyp) contents in liver tissue of the rats in 3 groups were determined with HCl hydrolysis, and collagen type I, transforming growth factor-beta 1 (TGF-beta1), transforming growth factor-beta receptor type I (TbetaRI) and transforming growth factor-beta receptor type II (TbetaRII) were detected by Western blotting. RESULTS: The Hyp content and the expressions of collagen type I, TGF-beta1, TbetaRI and TbetaRII in the liver tissue of rats in the untreated group increased significantly as compared with those in the normal control group, while those in SA-B-treated group decreased significantly as compared with those in the untreated group. CONCLUSION: The therapeutic mechanism of SA-B in treating hepatic fibrosis may be related to inhibiting the expressions of TGF-beta1 and its receptors.
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Objective:To study the chemical constituents of the peels collected from Citrus changshan-huyou Y.B.Chang,and further screen the bioactive components as the lead structures.Methods: These compounds were isolated by repeated flash column chromatography on silica gel and Sephadex LH-20.The structures of isolated compounds were elucidated by using IR,EIMS,and NMR analyses.Results: One novel compound along with nine known compounds were obtained and identified as huyoujiasu(Ⅰ),3-hydroxy-4-methoxybenzoic acid(Ⅱ),3,4-dihydroxybenzoic acid(Ⅲ),fatty acid(Ⅳ),gly-ceride(Ⅴ),6,7-dimethoxycoumarin(Ⅵ),6′,7′-dihydroxybergamottin(Ⅶ),daucossterol A(Ⅷ),daucossterol B(Ⅸ) and huyou-triterpenoid(Ⅹ).Conclusion: One new compound,Huyoujiasu,was obtained from these peels by repeated column chromatography,and the other known compounds were isolated from this fruit for the first time as well.
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Objective To further study on the chemical constituents in the peels of Citrus changshan-huyou.Methods The chemical constituents were separated by repeated silica gel column chromatography,the structures were determined by spectral analyses.Results Ten compounds were obtained and identified as huyoujiasu(2'-hydroxy-malonyl-3,4-dihydroxybenzoic acid,Ⅰ),3'-hydroxy-4',5,6,7,8-pentamethoxyflavone(Ⅱ),eriodictyol(Ⅲ),tetracosanoic acid(Ⅳ),glyceryl dodecanoate(Ⅴ),neoeriocitrin(Ⅵ),naringin(Ⅶ),neohesperidin(Ⅷ),4-methoxy-3-hydroxybenzoic acid(Ⅸ),and 3,4-dihydroxybenzoic acid(Ⅹ).Conclusion 2'-hydroxy-malonyl-3,4-dihydroxybenzoic acid is a new compound and the above ten compounds are obtained from this plant for the first time.
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Object A systematic study on the chemical constituents of Citrus changshan huyou Y B Chang was carried out in order to reveal the active components for their further development Methods By repeated silica gel chromatographic separation and spectral analysis the structures were determined Results Six compounds of the flavonoids were obtained and identified They were hesperidin (hysperetin 7 O rutonoside) (Ⅰ); naringenin (Ⅱ); nobiletin (3′, 4′, 5, 6, 7, 8 hexamethoxyflavone) (Ⅲ); tangertin (4′, 5, 6, 7, 8 pentamethoxyflavone) (Ⅳ); 5 hydroxy 3′, 4′, 6, 7, 8 pentamethoxyflavone (Ⅴ); 5 hydroxy 3′, 4′, 6, 7, 8 haxamethoxyflavone (Ⅵ) Conclusion The above six compounds were obtained from this plant for the first time
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Objective: To develop a simple LC MS/MS method for the measurement of limonin in fructus evodiae, cortex phellodendri, cortex dictamni and its preparation. Methods: Separation was obtained by using a discovery C 18 column (150mm?2.1 mm), The mobile phase:A:water-0.1%HAc;B:acetonitrile-0.1%HAc;The elution program was gradient and the flow rate was 0.2mL?min -1 . The mass detector was set MS1(IS)=187.0 and MS2(Limonin)=471.0 by multiple reaction monitor(MRM) respectively.The sample was added psoralen(IS), then extracted with methanol chloroform(1∶3).Results: Limonin was linear from 25 to 1000ng?mL -1 ( r = 0.9996), The regression equation was C=3.124 As/Ai 1.935?10 -3 . The average recovery was 100.2%.Conclusion: This method is simple, quick, sensitive and exclusive.