Two new saponins 3-O-β-d-glucopyranosyl (1 → 2)-β-d-mannopyranosyl sarsasapogenin, named timosaponin A IV(1) and (5β, 25S)-26-O-β-d-glucopyranosyl-furost-20(22)-en-3,26-diol-3-O-β-d-glucopyranosyl (1 → 4) gluco...Two new saponins 3-O-β-d-glucopyranosyl (1 → 2)-β-d-mannopyranosyl sarsasapogenin, named timosaponin A IV(1) and (5β, 25S)-26-O-β-d-glucopyranosyl-furost-20(22)-en-3,26-diol-3-O-β-d-glucopyranosyl (1 → 4) glucopyranosyl (1 → 2)-β-d-galacopyranoside, named timosaponin B IV(2), were isolated by silica gel column chromatography and preparative HPLC from Anemarrhena asphodeloides Bge. Their structures were elucidated by chemical characters and spectroscopic analysis.展开更多
The objective of the research is to develop a quantitative method by ultra high-performance liquid chromatography/ quadrupole time-of-flight mass spectrometry （UHPLC/Q-TOF MS） for the analysis of seven major steroid...The objective of the research is to develop a quantitative method by ultra high-performance liquid chromatography/ quadrupole time-of-flight mass spectrometry （UHPLC/Q-TOF MS） for the analysis of seven major steroidal saponins （timosaponin N, timosaponin El, timosaponin BII, timosaponin B, anemarrhenasaponin I, anemarrhenasaponin A2, and timosaponin AIII） in Anemarrhena asphodeloides Bge. The complete separation of these seven steroidal saponins was achieved within 18 min with an ACQUITY UPLC HSS T3 column using an acetonitrile-water （contain 0.1% formic acid） gradient system. The limits of quantitation （LOQ）, 0.18-0.75 ng/pL for seven steroidal saponins, were determined experimentally. The limits of detection （LOD） were found to be 0.05-0.22 ng/μL for these saponins. The correlation coefficients （r2） for calibration curves varied from 0.9902 to 0.9979. This method showed good repeatability for the quantification of these saponins in rhizomes ofA. asphodeloides, with intra-day and inter-day variations of less than 5.0% for seven steroidal saponins. The recoveries of seven steroidal saponins were from 97.13% to 101.98%. The validated method was successfully applied to quantifying seven steroidal saponins in various sources ofA. asphodeloides （different collecting places or processing methods） and Zhimu concentrate-granules （ZMCG）.展开更多
Objective: To screen potential α-glucosidase inhibitors from Anemarrhena asphodeloides.Methods: Response surface methodology employing Box-Behnken design was used to optimize conditions for the extraction of α-gluco...Objective: To screen potential α-glucosidase inhibitors from Anemarrhena asphodeloides.Methods: Response surface methodology employing Box-Behnken design was used to optimize conditions for the extraction of α-glucosidase inhibitory active compounds from A. asphodeloides. The powders(20.0 g) of A. asphodeloides were extracted under the optimized conditions. The extract was applied to a D-101 macroporous resin column. It was eluted with ethanol and water to give six fractions. Compounds from the active fraction were identified by UPLC-Q-TOF-MS. The structure-activity relationship was discussed based on grey relational analysis.Results: The optimum extraction conditions were as follows: ethanol concentration, 100%; extraction temperature, 51 ℃; and solvent to solid ratio, 23 mL/g. It indicated that the active compounds were concentrated into 80% ethanol fraction. Twenty five steroid saponins from 80%ethanol fraction were identified by UPLC-Q-TOF-MS. Peaks 19 and 23 were tentatively identified as new structures. The predicted α-glucosidase inhibitory activities of the compounds were 7 > 2 > 1 > 22 > 23 > 3 > 9 > 21 > 24 > 4 > 13 > 8 > 14 > 16 > 17 > 25 > 6 > 19.Conclusion: The fraction eluted by 80% ethanol showed the best inhibitory activity. After analyzing the data of UPLC-Q-TOF-MS, 25 steroid saponins were tentatively identified in this fraction.展开更多
文摘Two new saponins 3-O-β-d-glucopyranosyl (1 → 2)-β-d-mannopyranosyl sarsasapogenin, named timosaponin A IV(1) and (5β, 25S)-26-O-β-d-glucopyranosyl-furost-20(22)-en-3,26-diol-3-O-β-d-glucopyranosyl (1 → 4) glucopyranosyl (1 → 2)-β-d-galacopyranoside, named timosaponin B IV(2), were isolated by silica gel column chromatography and preparative HPLC from Anemarrhena asphodeloides Bge. Their structures were elucidated by chemical characters and spectroscopic analysis.
基金Major National Science and Technology Projects (Grant No. 2009ZX09102-106, 2011ZX09102-002-09)National Natural Science Foundation of China (Grant No. 81274053)
文摘The objective of the research is to develop a quantitative method by ultra high-performance liquid chromatography/ quadrupole time-of-flight mass spectrometry （UHPLC/Q-TOF MS） for the analysis of seven major steroidal saponins （timosaponin N, timosaponin El, timosaponin BII, timosaponin B, anemarrhenasaponin I, anemarrhenasaponin A2, and timosaponin AIII） in Anemarrhena asphodeloides Bge. The complete separation of these seven steroidal saponins was achieved within 18 min with an ACQUITY UPLC HSS T3 column using an acetonitrile-water （contain 0.1% formic acid） gradient system. The limits of quantitation （LOQ）, 0.18-0.75 ng/pL for seven steroidal saponins, were determined experimentally. The limits of detection （LOD） were found to be 0.05-0.22 ng/μL for these saponins. The correlation coefficients （r2） for calibration curves varied from 0.9902 to 0.9979. This method showed good repeatability for the quantification of these saponins in rhizomes ofA. asphodeloides, with intra-day and inter-day variations of less than 5.0% for seven steroidal saponins. The recoveries of seven steroidal saponins were from 97.13% to 101.98%. The validated method was successfully applied to quantifying seven steroidal saponins in various sources ofA. asphodeloides （different collecting places or processing methods） and Zhimu concentrate-granules （ZMCG）.
基金the financial supports from Qiqihar Civic Scientific and Technological Project(SFGG-201559)
文摘Objective: To screen potential α-glucosidase inhibitors from Anemarrhena asphodeloides.Methods: Response surface methodology employing Box-Behnken design was used to optimize conditions for the extraction of α-glucosidase inhibitory active compounds from A. asphodeloides. The powders(20.0 g) of A. asphodeloides were extracted under the optimized conditions. The extract was applied to a D-101 macroporous resin column. It was eluted with ethanol and water to give six fractions. Compounds from the active fraction were identified by UPLC-Q-TOF-MS. The structure-activity relationship was discussed based on grey relational analysis.Results: The optimum extraction conditions were as follows: ethanol concentration, 100%; extraction temperature, 51 ℃; and solvent to solid ratio, 23 mL/g. It indicated that the active compounds were concentrated into 80% ethanol fraction. Twenty five steroid saponins from 80%ethanol fraction were identified by UPLC-Q-TOF-MS. Peaks 19 and 23 were tentatively identified as new structures. The predicted α-glucosidase inhibitory activities of the compounds were 7 > 2 > 1 > 22 > 23 > 3 > 9 > 21 > 24 > 4 > 13 > 8 > 14 > 16 > 17 > 25 > 6 > 19.Conclusion: The fraction eluted by 80% ethanol showed the best inhibitory activity. After analyzing the data of UPLC-Q-TOF-MS, 25 steroid saponins were tentatively identified in this fraction.
