目的:建立 RP-HPLC 法测定通光藤药材中11α-O-顺芷酰基-12β-O-乙酰基-通光藤苷元 B 的含量。方法:采用酸水解法降解通光藤 C_(21)甾体苷,以反相高效液相色谱法测定11α-O-顺芷酰基-12β-O-乙酰基-通光藤苷元 B 含量,色谱柱为 Diamonsi...目的:建立 RP-HPLC 法测定通光藤药材中11α-O-顺芷酰基-12β-O-乙酰基-通光藤苷元 B 的含量。方法:采用酸水解法降解通光藤 C_(21)甾体苷,以反相高效液相色谱法测定11α-O-顺芷酰基-12β-O-乙酰基-通光藤苷元 B 含量,色谱柱为 Diamonsil ODS(250 mm×4.6 mm,5 μm);柱温为16℃;流动相为乙腈-水(45:55);流速为0.8 mL·min^(-1);检测波长为220 nm。结果:11α-O-顺芷酰基-12β-O-乙酰基-通光藤苷元 B 进样量在1.016~5.080μg范围内与峰面积积分值呈良好的线性关系,r=0.9999(n=5);平均回收率(n=6)为98.8%,RSD=1.9%。结论:方法简便、快速、准确,为通光藤药材的质量评价和新药开发提供科学依据。展开更多
Progesterone(1) was biotransformed into the title compound 12β,15α-dihydroxy-progesterone(2) with Colletotrichum lini AS3.4486.The biotransformation process was monitored with HPLC.The structure of 2 was determi...Progesterone(1) was biotransformed into the title compound 12β,15α-dihydroxy-progesterone(2) with Colletotrichum lini AS3.4486.The biotransformation process was monitored with HPLC.The structure of 2 was determined by 1H NMR,13C NMR,ESI-MS and single-crystal X-ray diffraction.The crystal of the compound belongs to orthorhombic,space group P212121 with a = 8.0671(9),b = 12.3970(15),c = 18.532(3) ,Z = 4,V = 1853.3(4)3,Dc = 1.242 mg/m3,μ = 0.084 mm-1,F(000) = 752,R = 0.0373 and wR = 0.0850.Single-crystal X-ray diffraction analysis reveals that a 1D supramolecular structure of 2 has been constructed by multiply intermolecular O(2)-H(2)…O(4) and O(3)-H(3)…O(2) H-bonding interactions.展开更多
Gypenosides, a series of dammarane-type saponins from Gynostemma pentaphyllum Makino, were hydrolyzed under 5% H_2SO_4 catalysis to afford the title compound as a new secondary sapogenin in addition to panaxadiol and...Gypenosides, a series of dammarane-type saponins from Gynostemma pentaphyllum Makino, were hydrolyzed under 5% H_2SO_4 catalysis to afford the title compound as a new secondary sapogenin in addition to panaxadiol and 2a-hydroxypanaxadiol. The crystals of the title compound were obtained from methanol solution and a colourless crystal with dimensions of 0.2 × 0.2 × 0.2 mm was used. C_(30)H_(50)展开更多
基金supported by the Natural Science Foundation of Tianjin (Nos. 08JCZDJC15200 and 11JGYBJC14300)the Program for New Century Excellent Talents in University (No. NCET-08-0911)
文摘Progesterone(1) was biotransformed into the title compound 12β,15α-dihydroxy-progesterone(2) with Colletotrichum lini AS3.4486.The biotransformation process was monitored with HPLC.The structure of 2 was determined by 1H NMR,13C NMR,ESI-MS and single-crystal X-ray diffraction.The crystal of the compound belongs to orthorhombic,space group P212121 with a = 8.0671(9),b = 12.3970(15),c = 18.532(3) ,Z = 4,V = 1853.3(4)3,Dc = 1.242 mg/m3,μ = 0.084 mm-1,F(000) = 752,R = 0.0373 and wR = 0.0850.Single-crystal X-ray diffraction analysis reveals that a 1D supramolecular structure of 2 has been constructed by multiply intermolecular O(2)-H(2)…O(4) and O(3)-H(3)…O(2) H-bonding interactions.
文摘Gypenosides, a series of dammarane-type saponins from Gynostemma pentaphyllum Makino, were hydrolyzed under 5% H_2SO_4 catalysis to afford the title compound as a new secondary sapogenin in addition to panaxadiol and 2a-hydroxypanaxadiol. The crystals of the title compound were obtained from methanol solution and a colourless crystal with dimensions of 0.2 × 0.2 × 0.2 mm was used. C_(30)H_(50)