Aim A reliable and rapid HPLC method was developed for quantitative determination of coniferyl femlate, an ester of ferulic acid, with multiple pharmacological activities in Angelica sinensis and Ligusticum chuanxiong...Aim A reliable and rapid HPLC method was developed for quantitative determination of coniferyl femlate, an ester of ferulic acid, with multiple pharmacological activities in Angelica sinensis and Ligusticum chuanxiong, two commonly used Chinese medicines. Methods The determination was achieved by using a Zorbax ODS C18 analytical column （250 mm×4.6 mm ID, 5 μm） at isocratic elution of 1% aqueous acetic acid and acetonitrile （1：1） with diode-array detection （318 nm）. The calibration curve of coniferyl femlate showed good linearity （r^2 = 0.9995） within the test range. Results The developed method showed good precision with intra- and inter-day variations of 0.22% - 1.16% and 0.86% - 2.62% between the levels of 0.380 - 0.038 mg·mL^-1, respectively. The repeatability represented as RSD of coniferyl femlate was less than 2.7% for three levels （0.2 - 1.0 g of Angelica sinensis）, and the recovery was 105.3% with RSD of 3.2%. Conclusion The validated method was successfully applied to quantify coniferyl femlate in 12 samples of Danggui and Chuanxiong.展开更多
The reduction of 2,3-epoxy alcohol, prepared from the Sharpless asymmetric epoxidation, with the system of Ph3P, iodine, iwhdazole, 2,6-lutidine and water in Et2O/CH3CN,gives a chiral secondary allylic alcohol in 94% ...The reduction of 2,3-epoxy alcohol, prepared from the Sharpless asymmetric epoxidation, with the system of Ph3P, iodine, iwhdazole, 2,6-lutidine and water in Et2O/CH3CN,gives a chiral secondary allylic alcohol in 94% yield and 92% e.e.. Using this reaction as the key step, we synthesized (-)-coniferyl alcohol derivative 1 steding from the geraniol through nine steps in an overall yield of 39%.展开更多
Objective:To isolate and characterize chemical constituents of the roots of Zanthoxylumchalybeum(Z.chalybeum).Methods:A number of phytochemical tests were applied to identify the class of compounds present in the CH_(...Objective:To isolate and characterize chemical constituents of the roots of Zanthoxylumchalybeum(Z.chalybeum).Methods:A number of phytochemical tests were applied to identify the class of compounds present in the CH_(2)Cl_(2)/CH_(3)OH(1:1)root extract.Column chromatographic separation technique was applied to separate the constituents of the CH_(2)Cl_(2)/CH_(3)OH(1:1)root extract and various spectroscopic techniques[UV-vis,infrared radiation,nuclear magnetic resonance(NMR)(^(1)H-NMR,^(13)C NMR,DEPT-135,COSY,gHSQC and gHMBC)]were used to determine the structures of pure compounds.Results:Phytochemical screening of the CH_(2)Cl_(2)/CH_(3)OH(1:1)root extract of Z.chalybeum revealed the presence of alkaloids,flavonoids,terpenoids,tannins and anthraquinones.Column chromatographic separation of the extract yielded a new coniferyl alcohol derivative,2,3-epoxy-6,7-methylenedioxyconiferyl alcohol(1)together with the known alkaloid,dihydrochelerythrine(2).Conclusions:The present work conducted on the CH2Cl2:CH3OH(1:1)root extract of Z.chalybeum identified various class of compounds present in the root extract.Complete characterization of two compounds were done using spectroscopic techniques of which a coniferyl alcohol derivative(1)was identified for the first time.展开更多
基金Macao Science and Technology Development Fund(049/2005/A-R1) Jiangsu Key Laboratory for TCM FormulaeResearch, Nanjing University of Traditional Chinese Medicine (No.022021014003).
文摘Aim A reliable and rapid HPLC method was developed for quantitative determination of coniferyl femlate, an ester of ferulic acid, with multiple pharmacological activities in Angelica sinensis and Ligusticum chuanxiong, two commonly used Chinese medicines. Methods The determination was achieved by using a Zorbax ODS C18 analytical column （250 mm×4.6 mm ID, 5 μm） at isocratic elution of 1% aqueous acetic acid and acetonitrile （1：1） with diode-array detection （318 nm）. The calibration curve of coniferyl femlate showed good linearity （r^2 = 0.9995） within the test range. Results The developed method showed good precision with intra- and inter-day variations of 0.22% - 1.16% and 0.86% - 2.62% between the levels of 0.380 - 0.038 mg·mL^-1, respectively. The repeatability represented as RSD of coniferyl femlate was less than 2.7% for three levels （0.2 - 1.0 g of Angelica sinensis）, and the recovery was 105.3% with RSD of 3.2%. Conclusion The validated method was successfully applied to quantify coniferyl femlate in 12 samples of Danggui and Chuanxiong.
文摘The reduction of 2,3-epoxy alcohol, prepared from the Sharpless asymmetric epoxidation, with the system of Ph3P, iodine, iwhdazole, 2,6-lutidine and water in Et2O/CH3CN,gives a chiral secondary allylic alcohol in 94% yield and 92% e.e.. Using this reaction as the key step, we synthesized (-)-coniferyl alcohol derivative 1 steding from the geraniol through nine steps in an overall yield of 39%.
文摘Objective:To isolate and characterize chemical constituents of the roots of Zanthoxylumchalybeum(Z.chalybeum).Methods:A number of phytochemical tests were applied to identify the class of compounds present in the CH_(2)Cl_(2)/CH_(3)OH(1:1)root extract.Column chromatographic separation technique was applied to separate the constituents of the CH_(2)Cl_(2)/CH_(3)OH(1:1)root extract and various spectroscopic techniques[UV-vis,infrared radiation,nuclear magnetic resonance(NMR)(^(1)H-NMR,^(13)C NMR,DEPT-135,COSY,gHSQC and gHMBC)]were used to determine the structures of pure compounds.Results:Phytochemical screening of the CH_(2)Cl_(2)/CH_(3)OH(1:1)root extract of Z.chalybeum revealed the presence of alkaloids,flavonoids,terpenoids,tannins and anthraquinones.Column chromatographic separation of the extract yielded a new coniferyl alcohol derivative,2,3-epoxy-6,7-methylenedioxyconiferyl alcohol(1)together with the known alkaloid,dihydrochelerythrine(2).Conclusions:The present work conducted on the CH2Cl2:CH3OH(1:1)root extract of Z.chalybeum identified various class of compounds present in the root extract.Complete characterization of two compounds were done using spectroscopic techniques of which a coniferyl alcohol derivative(1)was identified for the first time.
