Preparation method of digital green intelligent high-purity marsdenia tenacissima component group and marsdenia tenacissima glycoside H and pharmaceutical composition thereof
A technology of vine vine glycoside and vine vine, which is applied in the field of digital, green, intelligent, high-purity vine vine glycoside and preparation of vine vine glycoside H and its pharmaceutical composition. Problems such as large loss of parts, to achieve the effects of shortening the production cycle, avoiding uneven quality, and reducing demand
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Embodiment 1
[0049] The preparation of embodiment 1 Tengguan rattan component group
[0050] 1) Extraction: Take 500g of Tengguan Teng powder, heat 4000ml of 30% ethanol solution, stir and extract quickly for 20min, centrifuge and filter while hot, heat 3000ml of 30% ethanol solution for filter residue 1, stir and extract quickly for 10min, centrifuge and filter while hot, and combine The two coarse filtrates were left to cool at room temperature for 2 hours, and filtered by intelligent cross-flow to obtain the fine filtrate. The fine filtrate is carried out to HPLC detection, and spectrogram sees figure 1 .
[0051] 2) Purification: Take the fine filtrate and pass it through the FL-2 macroporous adsorption resin column, wash it with 8BV of purified water, 8BV of 20% alcohol solution, 16BV of 30% alcohol solution, and 16BV of 40% alcohol solution until colorless or almost colorless, 3BV Elute with 50% ethanol solution, the flow rate is 1-2BV / h, collect the ethanol eluate that meets the t...
Embodiment 2
[0052] Example 2 The preparation of glucoside H
[0053] Take an appropriate amount of the above-mentioned preliminarily purified vine component group solution, pass through a C18 alkyl bonded silica gel column, wash and / or elute with 46% acetonitrile solution, collect vine glycoside H (area normalized Purity≧98.5%) eluate, acetonitrile is recovered under reduced pressure at 45°C to obtain a glucoside H solution, which is spray-dried under negative pressure to obtain an off-white powdered glucoside H with a purity of 99.22% and a yield of 95.59%. Chrysanthemum glucoside H is detected by HPLC according to the method of Example 1, and the spectrogram is shown in image 3 , the same method was used to detect the reference substance of guanvine glucoside H by HPLC, and the spectrum is shown in Figure 4 . After comparison with the spectrum of the reference substance, the sample is consistent with the reference substance, and the color is the same.
Embodiment 3
[0054] Example 3 The preparation of the active ingredient group of Tengguanteng
[0055] 1) Extraction Take 10kg of Tengguan rattan powder, heat 80kg of 30% ethanol solution, stir and extract quickly for 20min, centrifugally filter while hot, heat 60kg of 30% ethanol aqueous solution for filter residue 1, stir and extract quickly for 10min, centrifugally filter while hot, combine the two The crude filtrate was shaken and filtered for the first time, left to cool at room temperature for 2 hours, and filtered through intelligent cross-flow to obtain the fine filtrate.
[0056] 2) Purification: Take the fine filtrate and pass it through the FL-2 macroporous adsorption resin column, wash it with 8BV of purified water, 8BV of 20% alcohol solution, 16BV of 30% alcohol solution, and 16BV of 40% alcohol solution until colorless or almost colorless, 3BV 50% ethanol solution elution, flow rate 1-2BV / h, collect the eluate that meets the target requirements according to the set technical ...
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