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
The optimal conditions of the conversion of 16α methyl 3β,17α,21 trihydroxy 5α pregnane 20 one 21 acetate to 16α methyl 11α,17α,21 trihydroxy 1,4 pregndiene 3,20 dione by the mixed cultures of Arthrobacter sp 8...The optimal conditions of the conversion of 16α methyl 3β,17α,21 trihydroxy 5α pregnane 20 one 21 acetate to 16α methyl 11α,17α,21 trihydroxy 1,4 pregndiene 3,20 dione by the mixed cultures of Arthrobacter sp 86 and Metarhizium sp 88 were studied.2%～4%( V/V )N,N dimethylformamide in the medium was used to dissolve the substrate.It could increase the conversion ability.Adding the mycelium of Metarhizium into the dehydrogenation reaction mixture during 0～28 hours had no influence on the conversion rate.The optimal concentration of mycelium was around 75 mg/mL wet weight.0.04%～0.06% CoCl 2·6H 2O inhibited the degradation of steroid nucleus so that the product was greatly accumulated.Under such condition the yeild of mixed microbial conversion was 67%.展开更多
Two kinds of micro organism, Arthrobacter sp. AX86(1,4 dehdrogenator)and Absidia sp. A28(11α hydroxylator)were used in this experiment.Two different fermentation techniques were performed to accomplish the multiple c...Two kinds of micro organism, Arthrobacter sp. AX86(1,4 dehdrogenator)and Absidia sp. A28(11α hydroxylator)were used in this experiment.Two different fermentation techniques were performed to accomplish the multiple conversional reactions for producing 16β methyl 11α,17α,21 trihydroxy 1,4 pregnadiene 3,20 dione(Ⅲ)from 16β methyl 3β,17α,21 trihydroxy 5α pregnane 20 one 21 acetate(I):1)To produce product(Ⅲ)by means of a two step fermentation method which were independently performed first by Arthrobacter and next by Absiaia, and 2)the product was obtained by a sequential fermentation system of aforesaid two micro organisms in a single fermentor without isolation of the intermediates from the mixture.Our results showed that in both fermentation systems high yield of product was obtained.However,according to the technical simplicity,shorter duration of fermentation cycle and efficient yield of product,the second method is better than the first one.展开更多
The effects of solvent and impurity on the crystal habit of 11α-hydroxy-16α,17α-epoxyprogesterone (HEP)grown from solution were studied by scanning electron microscope.Long prismatic crystals were produced when HEP...The effects of solvent and impurity on the crystal habit of 11α-hydroxy-16α,17α-epoxyprogesterone (HEP)grown from solution were studied by scanning electron microscope.Long prismatic crystals were produced when HEP was crystallized from pure acetone and N,N-dimethylformamide,while blocky crystals were produced from pure chloroform by cooling crystallization.One kind of isomorphic impurity,16α,17α-epoxyprogesterone(EP) was selected to examine its effect on the HEP crystal habit.When the content of EP in the mother liquor is very high(55.45%,solvent free basis),the habit of produced HEP crystals was greatly modified from prismatic to octa-hedral.The differential scanning calorimetry and X-ray powder diffraction analyses showed that the change of crystal habit was originated from the crystal structure modification.展开更多
文摘The optimal conditions of the conversion of 16α methyl 3β,17α,21 trihydroxy 5α pregnane 20 one 21 acetate to 16α methyl 11α,17α,21 trihydroxy 1,4 pregndiene 3,20 dione by the mixed cultures of Arthrobacter sp 86 and Metarhizium sp 88 were studied.2%～4%( V/V )N,N dimethylformamide in the medium was used to dissolve the substrate.It could increase the conversion ability.Adding the mycelium of Metarhizium into the dehydrogenation reaction mixture during 0～28 hours had no influence on the conversion rate.The optimal concentration of mycelium was around 75 mg/mL wet weight.0.04%～0.06% CoCl 2·6H 2O inhibited the degradation of steroid nucleus so that the product was greatly accumulated.Under such condition the yeild of mixed microbial conversion was 67%.
文摘Two kinds of micro organism, Arthrobacter sp. AX86(1,4 dehdrogenator)and Absidia sp. A28(11α hydroxylator)were used in this experiment.Two different fermentation techniques were performed to accomplish the multiple conversional reactions for producing 16β methyl 11α,17α,21 trihydroxy 1,4 pregnadiene 3,20 dione(Ⅲ)from 16β methyl 3β,17α,21 trihydroxy 5α pregnane 20 one 21 acetate(I):1)To produce product(Ⅲ)by means of a two step fermentation method which were independently performed first by Arthrobacter and next by Absiaia, and 2)the product was obtained by a sequential fermentation system of aforesaid two micro organisms in a single fermentor without isolation of the intermediates from the mixture.Our results showed that in both fermentation systems high yield of product was obtained.However,according to the technical simplicity,shorter duration of fermentation cycle and efficient yield of product,the second method is better than the first one.
文摘The effects of solvent and impurity on the crystal habit of 11α-hydroxy-16α,17α-epoxyprogesterone (HEP)grown from solution were studied by scanning electron microscope.Long prismatic crystals were produced when HEP was crystallized from pure acetone and N,N-dimethylformamide,while blocky crystals were produced from pure chloroform by cooling crystallization.One kind of isomorphic impurity,16α,17α-epoxyprogesterone(EP) was selected to examine its effect on the HEP crystal habit.When the content of EP in the mother liquor is very high(55.45%,solvent free basis),the habit of produced HEP crystals was greatly modified from prismatic to octa-hedral.The differential scanning calorimetry and X-ray powder diffraction analyses showed that the change of crystal habit was originated from the crystal structure modification.
