ABSTRACT
The paper describes the development of a simultaneous determination method for polar and non-polar ginsenosides in red ginseng with a reversed-phase high-performance liquid chromatography-pulsed amperometric detection method. This method could be applied directly without any pretreatment steps and enabled the performance of highly sensitive analysis within 1h. The detection (S/N=3) and quantification (S/N=10) limits for the ginsenosides ranged 0.02-0.10 ng and 0.1-0.3 ng, respectively. The linear regression coefficients ranged 0.9975-0.9998. Intra- and inter-day precisions were <9.91%. The mean recoveries ranged 98.08-103.06%. The total amount of ginsenosides in the hairy root of red ginseng was higher than that in the main root.
Subject(s)
Chromatography, Reverse-Phase/methods , Conductometry/methods , Ginsenosides/analysis , Panax/chemistry , Chromatography, Reverse-Phase/statistics & numerical data , Conductometry/statistics & numerical data , Ginsenosides/chemistry , Limit of Detection , Molecular Structure , Plant Roots/chemistryABSTRACT
A simple and sensitive reversed-phase (RP) HPLC coupled with pulsed amperometric detection (PAD) method was developed to determine the saikosaponin content in Bupleuri Radix or Caihu-shugan-san. Four saikosaponins in Bupleuri Radix and Caihu-shugan-san were extracted with a 6:4 solution of 10 mM sodium phosphate buffer (pH 8)/100% ethanol. Pulsed amperometric detection of carbohydrates in four major saikosaponins was highly sensitive when used with a water-acetonitrile gradient on an alkaline RP column with a post-column delivery system. The limits of detection (S/N=3) and of quantification (S/N=10) of saikosaponins were 0.01-0.02 and 0.03-0.05 µg/mL, respectively. The intra- and inter-day precision (RSDs) were each <9.7% and the average recoveries were 95.0-97.6% in Bupleuri Radix. This method can be used to analyze saikosaponins in Bupleuri Radix and Caihu-shugan-san.
Subject(s)
Bupleurum/chemistry , Chromatography, High Pressure Liquid/methods , Chromatography, Reverse-Phase/methods , Drugs, Chinese Herbal/analysis , Oleanolic Acid/analogs & derivatives , Saponins/analysis , Chromatography, High Pressure Liquid/instrumentation , Chromatography, Reverse-Phase/instrumentation , Oleanolic Acid/analysisABSTRACT
We developed a highly sensitive and selective reversed-phase HPLC-pulsed amperometric detection (RP-HPLC-PAD) method for cardiac glycoside detection. Eight cardiac glycosides were completely separated within 45 min on a reversed-phase column using a water-acetonitrile gradient, and were detected using a PAD under NaOH alkaline conditions. The detection (S/N=3) and quantification (S/N=10) limits for the cardiac glycosides were 0.1-0.3 and 0.3-0.8 ng, respectively. The linear regression coefficient was 0.9962-0.9998 for concentrations of 1-25 µg/mL. Cardiac glycosides in the Digitalis purpurea leaf displayed intra- and inter-day precisions (RSDs) of <9.30% and average recoveries of 98.63-99.94%. The contents of gitoxin, digitonin, and digitoxin in the D. purpurea were 0.197, 0.11, and 0.379 mg/g for leaf dried at 60 °C, 0.058, 0.11, and 0.090 mg/g for leaf dried at ambient temperature, and N.D. (not detected), and 18.379 mg/g, N.D. for seed, respectively. We conclude that our method shows good precision and accuracy.
Subject(s)
Chemistry Techniques, Analytical , Chromatography, High Pressure Liquid/methods , Digitalis/metabolism , Electrochemistry/methods , Acetonitriles/chemistry , Cardiac Glycosides/chemistry , Chemistry, Pharmaceutical/methods , Digitonin/analysis , Digitoxin/analysis , Digoxin/analogs & derivatives , Digoxin/analysis , Models, Chemical , Plant Leaves/metabolism , Reproducibility of Results , Solvents , TemperatureABSTRACT
The methanolic extract of the roots of Polygonum multiflorum (Polygonaceae) was found to show inhibitory activity towards farnesyl protein transferase (FPTase). Bioassay-guided fractionation of the methanolic extract resulted in the isolation of two anthraquinone glycosides, as inhibitors of FPTase. These compounds inhibited the FPTase activity in a dose-dependent manner.
Subject(s)
Alkyl and Aryl Transferases/antagonists & inhibitors , Anthraquinones/pharmacology , Enzyme Inhibitors/pharmacology , Glycosides/pharmacology , Polygonum , Anthraquinones/chemistry , Anthraquinones/isolation & purification , Biological Assay , Chemical Fractionation , Dose-Response Relationship, Drug , Enzyme Inhibitors/chemistry , Enzyme Inhibitors/isolation & purification , Glycosides/chemistry , Glycosides/isolation & purification , Methanol/chemistry , Molecular Structure , Plant Roots , Polygonum/chemistry , Solvents/chemistryABSTRACT
Five compounds were isolated from the chloroform-soluble fraction of the methanolic extract of the dried rhizomes of Zingiber officinale (Zingiberaceae) through repeated column chromatography. Their chemical structures were elucidated as 4-, 6-, 8-, and 10-gingerols, and 6-shogaol using spectroscopic analysis. Among the five isolated compounds, 6-shogaol exhibited the most potent cytotoxicity against human A549, SK-OV-3, SK-MEL-2, and HCT15 tumor cells. 6-shogaol inhibited proliferation of the transgenic mouse ovarian cancer cell lines, C1 (genotype: p53(-/-), c-myc, K-ras) and C2 (genotype: p53(-/-), c-myc, Akt), with ED(50) values of 0.58 microM (C1) and 10.7 microM (C2).
