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The preliminary metabolic profile of total diterpene acid (TDA) isolated from Pseudolarix kaempferi was investigated by using in vivo and in vitro tests. Pseudolaric acid C2 (PC2) was identified as the predominant metabolite in plasma, urine, bile and feces after both oral and intravenous administrations to rats using HPLC-UV and HPLC-ESI/MS(n), and demethoxydeacetoxypseudolaric acid B (DDPB), a metabolite proposed to be the glucoside of PC2 (PC2G), as well as pseudolaric acid C (PC), pseudolaric acid A (PA), pseudolaric acid A O-beta-D glucopyranoside (PAG), pseudolaric acid B O-beta-D glucopyranoside (PBG) and deacetylpseudolaric acid A (DPA) originated from TDA could also be detected. It was demonstrated by tests that the metabolism of TDA is independent of intestinal microflora, and neither of pepsin and trypsin is in charge of metabolism of TDA, TDA is also stable in both pH environments of gastric tract and intestinal tract. The metabolites of TDA in whole blood in vitro incubation were found to be PC2, DDPB and PC2G, which demonstrated that the metabolic reaction of TDA in vivo is mainly occurred in blood and contributed to be the hydrolysis of plasma esterase to ester bond, as well as the glucosylation reaction. These results clarified the metabolic pathway of TDA for the first time, which is of great significance to the in vivo active form and acting mechanism research of P. kaempferi.
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A new UPLC method was developed for the simultaneous determination of eleven characteristic flavonoid glycosides in Ginkgo biloba leaves. The natural occurrence of flavonoid glycosides in Ginkgo biloba leaves within one vegetative season was investigated for the first time. The analysis was performed on an Agilent ZORBAX Eclipse Plus C18 column (50 mm x 4.6 mm, 1.8 microm), the mobile phase A was acetonitrile, the mobile phase B was 0.4% phosphate aqueous solution in a gradient elution at a flow rate of 0.6 mL x min(-1), the detection was carried out at 360 nm. The result showed that eleven flavonoid glycosides had good linearity with good average recovery, separately. The method was proved to be accurate, rapid and good reproducible for the quality evaluation of Ginkgo biloba leaves, and provide an easy and rapid means for the quantitative analysis of flavonoid glycosides and their content fluctuation with seasons.
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Fragmentation behavior of diterpenoids was investigated by ESI/MSn and the qualitative analysis of diterpenoids in the bark of Pseudolarix kaempferi was performed using high-performance liquid chromatography/ multi-stage mass spectrometry (HPLC-ESI/MSn). The characteristic fragmentation behaviors of the diterpenoids are the cleavages of the lactone ring and C4-O bond. Furthermore, the eliminations of substituent groups at C-18, C-7 and C-8 can also be observed in the MS" (n = 3-4) spectra. For C-4 acetoxy subsititued diterpenoids, [M+Na-60]+ and [M-H-104] are the base peaks of MS2 spectra in the positive and negative ionization modes, respectively. For C-4 hydroxyl subsititued diterpenoids, [M+Na-44]+ and [M-H-62] are the base peaks of MS2 in the positive and negative ionization modes, respectively. For C-18 glucosylated or esterized diterpenoids, [M+Na-44]+ is the base peak of MS2 spectra in positive ionization mode. These fragmentation rules were successfully exploited in the identification of diterpenoids in methanol/water (6:4) extract of P. kaempferi by LC-MS in positive ionization mode. A total of 9 diterpenoids were identified or tentatively characterized, and one of them is reported here for the first time. The described method could be utilized for the sensitive and rapid qualitative analysis of P. kaempferi.
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The metabolic profile of pseudolaric acid B (PB) was investigated by using in vivo and in vitro tests. Pseudolaric acid C2 (PC2) was identified as the specific metabolite of PB in plasma, urine, bile and feces using HPLC and HPLC-ESI/MS(n) after both oral and intravenous administration to rats, and almost no prototype was detected in all kinds of samples. The metabolic behaviors of PB orally administered in rats treated with antibiotics to eliminate intestinal microflora were identical with those in untreated rats, demonstrating that the metabolism of PB is independent of intestinal microflora. PB was stable in 48 h respective incubation with artificial gastric juice and artificial intestinal juice, suggesting that neither pepsin nor trypsin is in charge of metabolism of PB, and also demonstrating that PB is stable in both pH environments of gastric tract and intestinal tract. In vitro research on metabolism of PB in rat liver microsomes incubation revealed that little PB was metabolized and that the proposed metabolites were the demethoxy and demethoxydecarboxy products of the prototype. The amount of metabolites was extremely low compared with the prototype, indicating that liver microsomes are not responsible for the metabolism of PB either. PB was gradually metabolized into PC2 during 1 h in whole blood incubation in vitro, and the metabolic process showed dynamically dependent manner with incubation time. Once absorbed into blood, PB was quickly metabolized into PC2, accordingly, little prototype was detected in all kinds of samples. The metabolism was attributed to the rapid hydrolysis of C-19 ester bond by plasma esterase. These results clarified the metabolic pathway of PB for the first time, which was of great significance to identify the in vivo active form and interpret acting mechanism of the active compounds of P. kaempferi.
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<p><b>OBJECTIVE</b>To establish a quantitative method with precolumn derivatization for determining the contents of six common amino acids in Banlangen Keli by UPLC.</p><p><b>METHOD</b>Using 6-acetamido-4-hydroxy-2-methyl quinoline as the derivating agent, we determined the contents of arginine, threonine , alanine, gamma aminobutyric acid, proline, and valine. The UPLC analysis was performed on a Waters AccQ Tag TM Ultra C18 column (2.1 mm x 100 mm, 5 microm) with mobile phase AccQ Tag Ultra Eluent A and AccQ Tag Ultra Eluent B gradient elution at a flow rate of 0.7 mL x min(-1). The column temperature was 55 degrees C and detection wavelength was 260 nm.</p><p><b>RESULT</b>The linear ranges of arginine, thremine, alanine, gamma aminobutyric acid, proline, and valine were 4. 15549.86 microg (r = 0.999 9), 0.595-5.95 microg (r = 0.999 8), 0.445-4.45 microg (r = 0. 999 9), 0.515-5. 15 pg (r = 0.999 9), 8.858-106.3 microg (r = 0.999 9) , 0.585-5. 85 microg (r = 0.999 8). Their average recoveries were 100.6%, 98.35%, 100.2%, 98.44%, 98.34%, 98.18% with RSD 1.8%,1.9%, 2.0%, 2.4%, 1.5% and 2.0%, respectively (n = 6). The contents of amino acids were different in samples from five productive enterprises.</p><p><b>CONCLUSION</b>The method is efficient, good reproducible, sensitive, and accurate.</p>
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Aminoácidos , Cromatografía Liquida , Medicamentos Herbarios Chinos , Química , Reproducibilidad de los ResultadosRESUMEN
The latest results from our research group in the biotransformation of triptolides and bufadienolides were reviewed. The trends in the development of biotransformation in the future were also briefly discussed.
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Objective:To observe the effect of liquiritin on body weight and behavior in depression model rats.Methods:Seventy-two male Sprague-Dawley(SD)rats were randomly assigned into normal control group,model group(stress+vehicle),fluoxetine group(stress+ fluoxetine)and three liquiritin groups(stress+liquiritin at different dose).The behavior of rats was detected by sucrose consumption test and forced swimming test.Results:The model rats showed significantly lower body weight(429?45/494?37,P
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Object To investigate the chemical constituents of Buddlejae officinalis Maxim. , the relationship between their bioactivities, and the medicinal application of the herb. Methods Various chro-matographic techniques were employed for the isolation and purification of the constituents, including silica gel, Sephadex LH-20, and pre-HPLC. The structures of 11 isolated chemical compounds were elucidated by chemical and spectral analysis (NMR, IR, UV, and MS). The aldose reductase inhibiting test and test on DNA topoisomerase Ⅳ inhibitory effect were applied to evaluate the bioactivity of both the purified compounds and the crude fraction. Results Eleven compounds were isolated from the extracts of B. offic-inalis. They are four flavones and their glycosides; apigenin (Ⅰ), linarin (Ⅱ), apigenin-7-O-?-L-rhamnopyranosyl (1-6)-?-D-glucopyranoside (Ⅲ), and luteolin-7-O-?-D-glucoside (Ⅶ); four phenylen-thanoid glycosides: verbascoside (Ⅴ), isoacteoside (Ⅵ), cistanoside F, a and b (Ⅶ-1 and 2), campneo-side Ⅱ , a and b (Ⅷ-1 and 2); three triferpenoid saponins: mimengoside A (Ⅸ), mimengoside B (Ⅹ), songaroside A (Ⅺ). Some of the them (such as Ⅱ ,Ⅲ , and Ⅵ) showed the aldose reductase inhibitory activities with a higher inhibitory rate than that of quercetin (the positive control), others (such as Ⅰ,Ⅱ , Ⅴ, Ⅵ, and Ⅺ) displayed the inhibititory activities against the DNA topoisomerase Ⅳ . Conclusion Among all the isolated compounds, Ⅲ , Ⅶ-1 and 2, Ⅷ-1 and 2, and Ⅺ are separated for the first time both from the plant and the genus. Their bioactivities of bacteriostatic and against aldose reductase with DNA topoisomerase Ⅳ as target are tested for the first time and are related to the medicinal application of B. officinalis.
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Fo r known flavonoids were isolated from the aerial part of Limonium sinense (Girald )-Kuntze. On the basis of UY, 1HNMR, 13CNMR and FAB-MS spectroscopic analysis, they wereidentified as myricetin-3-O-6-D-glucoside (Ⅰ), myricetin-3-O-?-L-rhamnoside (Ⅱ), quercetin3 O ?-L-rhamnoside (Ⅲ) and quercetin (Ⅳ). This seemed to be the first report describing theirisolation from L. sinense.
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Objective To investigate the derivatives of ginsenoside sapogenins and their activities against HL-60 cells.Methods The total ginsenoside extract was treated by Smith degradation.All products were isolated by silica gel chromatography and purified by preparative HPLC.On the basis of 1D and 2D NMR data,structures were elucidated.The activity against HL-60 cells was measured by MTT method.Results Three compounds were isolated and identified as 20(S)-protopanaxadiol(PD),20(S)-protopanaxatriol(PT),and 24,25-en-3?,6?-dihydroxy-12,20-(1′-hydroxy) ethanedioxy-dammarane(1).Conclusion Compound 1,named 1′-hydroxy ethanedioxy PT,is a novel derivate of sapogenin with higher inhibitory activity against HL-60 cells than PD and PT.
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Objective To study the chemical constituents of Smilax china.Methods The compounds were isolated by silica gel,Sephadex LH-20,ODS chromatography,and semi-preparative HPLC.Their structures were elucidated on the basis of MS and NMR spectroscopic analyses.Results Seven flavonoids and four stilbenes were isolated and identified as dihydrokaempferol-5-O-?-D-glucoside(Ⅰ),engeletin (Ⅱ),isoengeletin(Ⅲ),dihydroquercetin-3-O-glycoside(Ⅳ),3,5,7,3',5'-pentahydroxy-flavanonol (Ⅴ),astilbin(Ⅵ),quercetin-3'-Oglycoside(Ⅶ),piceid(Ⅷ),scirpusin A(Ⅸ),resveratrol(Ⅹ),and oxyresveratrol(Ⅺ).Conclusion CompoundsⅣ—Ⅸare isolated from this plant for the first time,among which the ~(13)C-NMR data of compoundⅨis reported firstly.