A normal phase enantioselective high performance liquid chromatographic method was developed for enantiomeric resolution of Ezetimibe it reduces the overall delivery of cholesterol to the liver. The enantiomers of Eze...A normal phase enantioselective high performance liquid chromatographic method was developed for enantiomeric resolution of Ezetimibe it reduces the overall delivery of cholesterol to the liver. The enantiomers of Ezetimibe were resolved on a Chiral Pak AS-H (250 × 4.6 mm, 5 μm) column using a mobile phase system containing n-Hexane, etha-nol, 2-Propanol and Trifloroacetic acid (84:12:4:0.1 v/v). The resolution between enantiomers was found to be more than 2.0. The limit of detection and limit of quantification of (R)-enantiomer were found to be 0.2 μg/mL and 0.5 μg/mL, respectively, for 10 μL injection volume. The sample solution and mobile phase were found to be stable for at least 48 h. The final optimized method was successfully applied to separate (R)-enantiomer from Ezetimibe and was proven to be reproducible and accurate for the quantitative determination of (R)-enantiomer in bulk drugs.展开更多
目的:建立R-维格列汀的检测方法。方法:采用高效液相色谱法,色谱柱采用CHIRALPAK R IC手性柱(4.6mm×250mm,5μm),流动相为乙醇-二乙胺(100∶0.1),柱温:25℃,流速为0.5mL/min;检测波长为210nm;进样量10μL。结果:R-维格列汀的检测...目的:建立R-维格列汀的检测方法。方法:采用高效液相色谱法,色谱柱采用CHIRALPAK R IC手性柱(4.6mm×250mm,5μm),流动相为乙醇-二乙胺(100∶0.1),柱温:25℃,流速为0.5mL/min;检测波长为210nm;进样量10μL。结果:R-维格列汀的检测限和定量限分别为0.309μg/mL和1.236μg/mL,R-维格列汀在0.5～10.0μg/mL范围内线性关系良好(r=0.9996);平均回收率为100.12%(RSD=0.80%);4批样品检测结果表明,其R-维格列汀含量均低于检测限。结论:本方法操作简便、快捷,结果准确、可靠,可用于R-维格列汀的含量控制。展开更多
Objective:To study the chemical constituents of the roots of Angelica dahurica,a well-known Chinese herbal medicine named Baizhi in Chinese.Methods:Compounds were separated by various chromatographies,and the structur...Objective:To study the chemical constituents of the roots of Angelica dahurica,a well-known Chinese herbal medicine named Baizhi in Chinese.Methods:Compounds were separated by various chromatographies,and the structures of new compounds were elucidated based on the analysis of their spectroscopic and spectrometric data(1D,2D NMR,HRESI MS,IR,and UV).The absolute configurations of new compounds were determined by the calculated electronic circular dichroism and chemical derivatization.The inhibitory activities of all isolates against nitric oxide(NO)production were evaluated using lipopolysaccharide-activated RAW 264.7macrophage cells.Results:Seven new 3,4-dihydro-furanocoumarin derivatives(1a/1b,2a/2b,3a/3b,4)together with a known furanocoumarin(5)were isolated from the roots of A.dahurica.The new compounds included three pairs of enantiomers,(4S,2’’R)-angelicadin A(1a)/(4R,2’’S)-angelicadin A(1b),(4S,2’’S)-angelicadin A(2a)/(4R,2’’R)-angelicadin A(2b),and(4S,2’’S)-secoangelicadin A(3a)/(4R,2’’R)-secoangelicadin A(3b),together with(4R,2’’R)-secoangelicadin A methyl ester(4).The known xanthotoxol(5)inhibited the NO production with the half-maximal inhibitory concentration(IC50)value of(32.8±0.8)μmol/L,but all the new compounds showed no inhibitory activities at the concentration of100μmol/L.Conclusion:This is the first report of the discovery of 3,4-dihydro-furanocoumarins from A.dahurica.The results are not only meaningful for the understanding of the chemical constituents of A.dahurica,but also enrich the reservoir of natural products.展开更多
文摘A normal phase enantioselective high performance liquid chromatographic method was developed for enantiomeric resolution of Ezetimibe it reduces the overall delivery of cholesterol to the liver. The enantiomers of Ezetimibe were resolved on a Chiral Pak AS-H (250 × 4.6 mm, 5 μm) column using a mobile phase system containing n-Hexane, etha-nol, 2-Propanol and Trifloroacetic acid (84:12:4:0.1 v/v). The resolution between enantiomers was found to be more than 2.0. The limit of detection and limit of quantification of (R)-enantiomer were found to be 0.2 μg/mL and 0.5 μg/mL, respectively, for 10 μL injection volume. The sample solution and mobile phase were found to be stable for at least 48 h. The final optimized method was successfully applied to separate (R)-enantiomer from Ezetimibe and was proven to be reproducible and accurate for the quantitative determination of (R)-enantiomer in bulk drugs.
文摘目的:建立R-维格列汀的检测方法。方法:采用高效液相色谱法,色谱柱采用CHIRALPAK R IC手性柱(4.6mm×250mm,5μm),流动相为乙醇-二乙胺(100∶0.1),柱温:25℃,流速为0.5mL/min;检测波长为210nm;进样量10μL。结果:R-维格列汀的检测限和定量限分别为0.309μg/mL和1.236μg/mL,R-维格列汀在0.5～10.0μg/mL范围内线性关系良好(r=0.9996);平均回收率为100.12%(RSD=0.80%);4批样品检测结果表明,其R-维格列汀含量均低于检测限。结论:本方法操作简便、快捷,结果准确、可靠,可用于R-维格列汀的含量控制。
基金financially supported by Beijing Natural Science Foundation(No.7202125)。
文摘Objective:To study the chemical constituents of the roots of Angelica dahurica,a well-known Chinese herbal medicine named Baizhi in Chinese.Methods:Compounds were separated by various chromatographies,and the structures of new compounds were elucidated based on the analysis of their spectroscopic and spectrometric data(1D,2D NMR,HRESI MS,IR,and UV).The absolute configurations of new compounds were determined by the calculated electronic circular dichroism and chemical derivatization.The inhibitory activities of all isolates against nitric oxide(NO)production were evaluated using lipopolysaccharide-activated RAW 264.7macrophage cells.Results:Seven new 3,4-dihydro-furanocoumarin derivatives(1a/1b,2a/2b,3a/3b,4)together with a known furanocoumarin(5)were isolated from the roots of A.dahurica.The new compounds included three pairs of enantiomers,(4S,2’’R)-angelicadin A(1a)/(4R,2’’S)-angelicadin A(1b),(4S,2’’S)-angelicadin A(2a)/(4R,2’’R)-angelicadin A(2b),and(4S,2’’S)-secoangelicadin A(3a)/(4R,2’’R)-secoangelicadin A(3b),together with(4R,2’’R)-secoangelicadin A methyl ester(4).The known xanthotoxol(5)inhibited the NO production with the half-maximal inhibitory concentration(IC50)value of(32.8±0.8)μmol/L,but all the new compounds showed no inhibitory activities at the concentration of100μmol/L.Conclusion:This is the first report of the discovery of 3,4-dihydro-furanocoumarins from A.dahurica.The results are not only meaningful for the understanding of the chemical constituents of A.dahurica,but also enrich the reservoir of natural products.
