Preparation method for eleutheroside
A technique for total glycosides of Acanthopanax senticosus and chromatography, which can be applied to chemical instruments and methods, medical preparations containing active ingredients, glycosides, etc., and can solve problems such as complex methods and the like.
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Embodiment 1
[0071] Example 1: Purify eleutherosides by gradient elution method, and optimize the concentration parameters of the eluent:
[0072] (1) Adopt existing technology to extract 28kg Acanthopanax, get 35L Acanthopanax extract, which is Acanthopanax aqueous extract, dissolve Acanthopanax aqueous extract with a small amount of methanol, ultrasonically make the dissolution even, use 0.45 μm microporous membrane filtration, the obtained filtrate is used for later use;
[0073] (2) Under normal temperature and pressure, use HPD-450 type macroporous adsorption resin as the stationary phase, fill the column with the stationary phase, and then use the macroporous resin column chromatography to separate the filtrate obtained in step (1), using 10% volume percentage in turn , 20%, 30%, 40%, 50%, 60%, 70%, 80%, 90% ethanol aqueous solution for elution, the amount of each concentration of ethanol aqueous solution is 3 to 4 times the column volume, collect each The eluent corresponding to th...
Embodiment 2
[0080] Embodiment two: Small scale scale-up experiment
[0081] Take 5kg of HPD-450 macroporous resin and pack it into a column. After pretreatment, wash with water until neutral. The column volume is 7L. Take 6.5L (184.6g alcohol extract) of Acanthopanax acanthopanax extract, and wash it with water, 20% by volume, and 30% ethanol aqueous solution in turn, and the volume of the eluent is 21L (3 column volumes). Concentrations of ethanol-water corresponding eluate fractions.
[0082] Then, as in Example 1, high performance liquid chromatography is used to analyze and detect the fractions corresponding to the eluents of each concentration. The difference is that the detection wavelengths are 203nm and 265nm; the results can be found in Figure 10-15 , it can be seen from the figure that 20% ethanol can not completely wash off the desired substance, and it is also demonstrated after repeated washing with 20% ethanol afterwards.
Embodiment 3
[0083] Embodiment 3: Small scale scale-up experiment (the eluting solution is ethanol aqueous solution with a volume fraction of 30%)
[0084] Take 5kg of HPD-450 macroporous resin and pack it into a column. After pretreatment, wash with water until neutral. The column volume is 7L. Take 6.5L (184.6g alcohol extract) of Acanthopanax acanthopanax extract, elute continuously with 30% by volume ethanol aqueous solution, collect the eluate fractions of each column volume respectively, and repeat 6 groups; then Each fraction is analyzed and detected, the detection method is with reference to Example 1, the detection wavelength is 203nm and 265nm, the results can be found in Figures 26-50 , it is known from the figure that the elution with 30% ethanol concentration is stable.
[0085] The 30% ethanol of the 2nd column volume in the embodiment is the high-performance liquid chromatogram of eluent corresponding fraction is analyzed, adopts absorbance method to quantitatively analyze...
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