Method for preparing chemical reference substance semen momordicae saponin I with high purity
A high-purity, wood turtle technology is applied in chemical instruments and methods, organic chemistry, preparation of sugar derivatives, etc. It can solve the problems of low yield and cumbersome operation, achieve high yield, simplify the preparation process, and improve yield. rate effect
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Embodiment 1
[0030] This embodiment 1 is implemented under the following conditions of implementation and technical requirements:
[0031] 1. Add 200g of wood turtle seeds, add 1600mL water to decoct twice, each time for 0.5h, centrifuge, take the supernatant, and concentrate the supernatant to 250mL for later use.
[0032] 2. Add 250 mL of ethyl acetate to the supernatant and extract twice, recover the ethyl acetate, discard the extract; evaporate the lower aqueous solution on a water bath until there is no ethyl acetate smell, and obtain an aqueous solution.
[0033] 3. On the D101 macroporous resin column (400g resin) in the aqueous solution, first wash 4 column volumes with water, then use 20% ethanol to elute 4 column volumes, and then 50% ethanol to elute 4 column volumes (the flow rate is 0.4BV / h). Collect 50% ethanol eluate (each fraction 0.4BV), reverse phase TLC detection, merge the fractions with the same main spot (Rf0.20‐0.25), recover ethanol (can be used again) to obtain t...
Embodiment 2
[0037] This embodiment 2 is implemented under the following conditions of implementation and technical requirements:
[0038] 1. Add 200g of wood turtle seeds, add 2L of water and decoct twice, 45 minutes each time, centrifuge the extract, take the supernatant, and concentrate the supernatant to 220mL.
[0039] 2. Add 220 mL of ethyl acetate to the aqueous solution for extraction three times, and recover the ethyl acetate under reduced pressure. The water layer was placed on a water bath and the ethyl acetate was evaporated to obtain an aqueous solution.
[0040]3. Put the aqueous solution on D101 macroporous resin column (500g resin, flow rate is 0.4BV / h), first wash 5 column volumes with water, then use 25% ethanol to elute 5 column volumes, and then 50% ethanol to elute 5 columns volume. Collect 50% ethanol eluate (each fraction 0.4BV), reverse phase TLC detection, merge the fractions with the same main spot (Rf0.20‐0.25), recover ethanol (can be used again) to obtain the...
Embodiment 3
[0044] This embodiment 3 is implemented under the following conditions of implementation and technical requirements:
[0045] 1. Add 2.4L of water to decoct 200g of wood turtle seeds for 3 times, 60 minutes each time, centrifuge the extract, take the supernatant, and concentrate to 200mL.
[0046] 2. Add 200 mL of ethyl acetate to the aqueous solution to extract 3 times, and recover the ethyl acetate under reduced pressure. The water layer was placed on a water bath and the ethyl acetate was evaporated to obtain an aqueous solution.
[0047] 3. Put the D101 macroporous resin column (600g resin, the flow rate is 0.4BV / h) on the aqueous solution, first wash 6 column volumes with water, then elute 6 column volumes with 25% ethanol, and then elute 6 column volumes with 50% ethanol column volume. Collect 50% ethanol eluate (each fraction 0.4BV), reversed-phase TLC detection, merge the fractions with the same main spot (Rf0.20‐0.25), recover ethanol to obtain the extract of magnol...
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