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OBJECTIVE：To establish the method for content dete rmination of polyphyllin Ⅱ，Ⅵ，Ⅶ in Ypsilandra thibetica ， and to compare the differences of 3 saponins in different parts of Y. thibetica from different producing areas. METHODS ：HPLC method was adopted to determine the contents of polyphyllin Ⅱ，Ⅵ，Ⅶ in whole grass part and underground part of Y. thibetica from 10 producing areas. The determination was performed on Kromasil C 18column with mobile phase consisted of acetonirile-water （gradient elution ）at the flow rate of 1.0 mL/min. The column temperature was 35 ℃，and detection wavelength was set at 203 nm；sample size was 10 μL. With the contents of 3 saponins as the index ，20 batches of Y. thibetica were analyzed by cluster analysis and PLS-DA analysis ；the aggregation of samples was analyzed and determined the primary difference components. RESULTS：The linear range of polyphyllin Ⅱ，polyphyllin Ⅵ and polyphyllin Ⅶ were 0.051-2.04，0.007-0.28，0.168-6.72 μg， respectively（r≥0.999 5）；the detection limits were 1.92，1.75，1.87 ng，respectively；and the quantitative limits were 6.40，5.87， 6.23 ng，respectively；RSD of precision ，reproducibility and stability tests （24 h）were all lower than 2％（n＝6）；the average recovery rates were 99.29％，101.38％ and 99.64％，with RSDs of 1.17％，2.64％，0.75％（n＝6），respectively. The content of polyphyllin Ⅱ was 0.615-1.875 mg/g，that of polyphyllin Ⅵ was 0-0.095 mg/g，and that of polyphyllin Ⅶ was 3.158-12.354 mg/g. Cluster analysis showed that 20 batches of samples were clustered into two groups ，batch S 9-S12 were clustered in to one group，and the other 16 batches of samples were clustered into another group. PLS-DA analysis showed that 20 batches of samples were divided into 3 areas，batch S 1，S2，S8，S14，S16，S20 were included in area Ⅰ；batch S 9-S12 included in area Ⅱ；and the rest of the samples included in area Ⅲ. The quality of Y. thibetica from different habitats was different ，and there was no difference in the saponin composition between the whole grass and the underground part. Weight ranking found that mail：cscdtcm@126.com polyphyllin Ⅶ was the main difference component in Y. thibetica，and the content of polyphyllin Ⅶ in Y. thibetica from Pengzhou city and Dayi county was the highest. CONCLUSIONS ：The established method is simple ，convenient and sensitive. It can be used for the content determination of 3 saponins in Y. thibetica . The content of active components is higher and the quality is better in Y. thibetica from Pengzhou city and Dayi county.
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OBJECTIVE： To conduct structural modification of tectorigenin to search for new compounds with anti-tumor activity. METHODS： Tectorigenin was used as a lead compound， and then added into amine reagents as ethanolamine， methylamine， ethylamine， dimethylamine， diethylamine， n-propylamine and formaldehyde solution. Tectorigenin Mannich base derivatives were synthesized by mannich reaction with as the lead compound. The structures of the derivatives were identified according to IR， UV， MS and NMR data. Solubility of tectorigenin and its derivatives were investigated by solubility test method. MTT assay was used to investigate the inhibitory effects of tectorigenin and its derivatives on the proliferation of human colon cancer cell line HCT116， human lung cancer cell line A549 and human hepatoma cell line HepG2， and half inhibitory concentration （IC50） was calculated. The inhibition rate of tectorigenin and its derivatives （100 mg/kg） on H22 hepatoma-bearing mice in vivo was studied. RESULTS： Totally of 6 kinds of tectorigenin mannich base derivatives were synthesized， such as 8-（N-hydroxyethyl）-methyleneamino-5，7，4′-trihydroxy-6-methoxyisoflavone， 8-（N-methyl）-methyleneamino-5，7，4′-trihydroxy-6- methoxyisoflavone， 8-（N， N-diethyl）-methyleneamino-5，7，4′-trihydroxy-6-methoxyisoflavone， 8-（N， N-dimethyl）-methyleneamino- 5，7，4′-trihydroxy-6-methoxyisoflavone， 8-（N-ethyl）-methyleneamino-5，7，4′-trihydroxy-6-methoxyisoflavone， 8-（N-propyl）- methyleneamino-5，7，4′-trihydroxy-6-methoxyisoflavone （compounds 1-6 in turn）. Compared with tectorigenin， the water solubility of six derivatives was significantly improved， and the solubility was 5-20 times higher than that of tectorigenin. IC50 of compounds 1， 3 and 5 to HCT116 cells were （34.82±3.27）， （16.21±4.13）， （33.12±3.25） μmol/L， which were stronger than that of tectorigenin [（45.23±5.74） μmol/L]； IC50 of compounds 1， 3 and 5 to A549 cells were （37.05±5.74）， （26.88±4.52）， （30.13±6.23） μmol/L， which were stronger than that of tectorigenin [（53.24±6.34） μmol/L]； IC50 of compounds 1， 3 and 5 to HepG2 cells were （23.74±1.45）， （18.96±2.34）， （30.95±2.87） μmol/L， which were stronger than that of tectorigenin [（48.98±2.58） μmol/L]. Compounds 1， 3 and 5 showed higher inhibition rates （55.51％， 57.20％ and 49.15％） than tectorigenin （33.05％） on H22 hepatoma-bearing mice， respectively. The other three compounds had no obvious advantage over tectorigenin in anti-tumor activity. CONCLUSIONS： In this study， compounds 1， 3 and 5 of six tectorigenin mannich base derivatives synthesized in this study have stronger antitumor activity than tectorigenin.
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OBJECTIVE:To establish the quality standard of Belamcandin standard substance.METHODS:Different indices of standard Belamcandin were examined with quantitative and quantitative analyses according to the corresponding measures stipulated in the Appendix of pharmacopoeia of people's republic of China(part Ⅱ)published in 2005.RESULTS:The specific rotatory power of 3 batches of standard Belamcandin was —28?～—30?([?]25 D,c0.11,Pyridine);the E1% 1 cmwas 790～830;the melting point was 252～254 ℃ and the ash content was less than 0.5%.The content of Belamcandin in the products was above 99.5% as revealed by HPLC.CONCLUSION:All of the indices were shown to meet the standards for standard substances and the established standard can be used for the quality control of standard Belamcandin.
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Object To do detail investigation of the saponins from the Chinese materia medica Huluba (the seeds of Trigonella foenum graecum L ) Methods The pure saponins from the total saponins were isolated by employing the column chromatography and dry column chromatography of silica gel H Their chemical structures were elucidated by 13 C NMR , FAB MS, DEPT spectroscopic evidence and the results of the fraction hydrolysis of acquiring their secondary glucosides were obtained Results Two new saponins B and C were isolated and both were the glucosides consisted by four molecules of sugar with diosgenin The chemical structure of B is: diosgenin 3 O ? L rhamnopyranosyl (1→3) ? L rhamnopyranosyl (1→4) ? D glucopyranosyl (1→4) ? D glucopyranoside And saponin C is: diosgenin 3 O ? D glucopyranosyl (1→4) ? L rhamnopyranosyl (1→4) ? D glucopyranosyl (1→4) ? D glucopyranoside Conclusion Saponins B and C are two new ones with four molecules of sugar respectively
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Object To investigate the saponin from the seeds of Trigonella foenum graecum Linn (STFG) Methods The total saponin from STFG was extracted and purified by using the absorptive resin, the single saponin was isolated by using the column chromatography as well as dry column chromatography of silica gel H The chemical structure was elucidated by 13 CNMR , FAB MS, DEPT spectroscopic evidence and the results of fraction hydrolysis of acquiring their secondary glucosides Results A new saponin A from the total saponin has been obtained, the fraction hydrolysis carried out and the secondary glucoside Ⅰ and Ⅱ identified by determining the structure of saponin A The chemical structure of saponin A is: diosgenin 3 O ? L rhamnopyranosyl(1→4) ? D glucopyranosyl(1→4) ? D glucopyranoside The secondary glucoside Ⅰ is: diosgenin 3 O ? D glucopyranoside; Ⅱ is: diosgenin 3 O ? D glucopyranosyl(1→4) ? D glucopyranoside Conclusion Glucoside A is a new saponin with three molecules of sugar
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Objective To investigate the saponins from the Chinese materia medica Huluba (the seeds of Trigonella foenum-graecum L.). Methods To isolate and purify the single saponin by the column chromatography and dry column chromatography of silica gel H. The structural elucidation was carried on by spectroscopic evidence of (()~(13)C-NMR), FAB-MS, DEPT and the results of the fraction-hydrolysis of acquiring the secondary glucosides. Results The newly isolated saponin D was consisted by six molecules of sugar with diosgenin. The chemical structure of saponin D is: diosgenin-3-O-?-L-rhamnopyranosyl (1→3)-?-D-glucopyranosyl (1→4)-?-L-rhamnopyranosyl [(1→3)-?-L-rhamnopyranosyl] (1→4)-?-D-glucopyranosyl (1→4)-?-D-glucopyranoside. Conclusion Saponin D is a new one consisted of six molecules of su-(gar) with diosgenin.
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OBJECTIVE:To determine the content of Tectoridin in Rhizoma Iridis Tectori by HPLC. METHODS: The chromatographic separation was performed on Diamond ODS C18 column(150 mm?4.6 mm,5 ?m) with mobile phase consisted of MeOH-0.5% acetic acid(3∶7) at a flow rate of 0.8 mL?min-1. The detection wavelength was set at 265 nm.RESULTS: Good linear relationship was achieved over the concentration range of 0.079 2～0.396 0 ?g for tectoridin with an average recovery of 99.80%(RSD=1.09%,n=6). CONCLUSION: The method is sensitive, simple and accurate, and it can be used for the quality control of Rhizoma Iridis Tectori.