A kind of compound and its preparation method and application
A technology for compounds and concentrates, applied in the field of compounds and their preparation, can solve problems such as systematic research that has not been reported
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[0039] The present invention also provides a method for preparing the compound of formula (I), including:
[0040] 1) Perform chromatographic separation of Dragon's blood through a macroporous adsorption resin column, eluting with an aqueous solution of alcohol with a first mass concentration and an aqueous solution of alcohol with a second mass concentration, and collect the elution parts of the aqueous solution of alcohol with a second mass concentration Eluent,
[0041] The alcohol is a C1-C6 alcohol,
[0042] The first mass concentration alcohol aqueous solution is 20% to 60% alcohol aqueous solution,
[0043] The second mass concentration of the alcohol aqueous solution is an 80% to 98% alcohol aqueous solution;
[0044] 2) Concentrate the eluate obtained in step 1) to obtain a concentrate of the second mass concentration of the eluted portion of the alcohol aqueous solution;
[0045] 3) Chromatographic separation of the concentrate obtained in step 2), and the collection contains ...
Embodiment 1
[0068] 10g of the raw material of Longxuetongluo Capsules was dissolved in 40% ethanol and loaded, separated by HP-20 macroporous adsorption resin chromatographic column, and eluted with 2L 40% alcohol aqueous solution, 2L 95% alcohol aqueous solution, and collected 95 The obtained eluate is eluted with a% alcohol aqueous solution, and the recovered eluate is concentrated to dryness to obtain a concentrate (extract I).
[0069] The extract I was dissolved in a small amount of methanol for LH-20 gel separation, the eluent was methanol, and 1 part (2mL) was automatically received every three minutes. A total of 30 components were collected, and the components 11-14 were combined and recorded as the group Part A is concentrated and dried.
[0070] Component A is dissolved in a small amount of methanol and then separated by LH-20 gel again. The eluent is methanol. One part (2mL) is automatically received every three minutes. A total of 30 components are collected, and each component A-...
Embodiment 2
[0075] 10g of dragon's blood total phenols were dissolved in 40% ethanol and loaded on HP-20 macroporous adsorption resin chromatographic column, followed by 1.5L 20% methanol aqueous solution, 1.5L 40% methanol aqueous solution, 1.5L 60% methanol aqueous solution, 1L 90 Elute with 5% methanol aqueous solution, collect the eluate obtained from 90% alcohol aqueous solution, and recover the eluate after concentrating to dryness to obtain a concentrate (Extract I).
[0076] The extract I was dissolved with a small amount of methanol to separate silica gel H, and the eluent was 500mL with chloroform: methanol volume ratio 15:1, 500mL 10:1, 500mL 5:1, 300mL 2:1, The TLC dot plate ultraviolet showed that the developing agent was chloroform: methanol 5:1, and a total of five components were collected and concentrated. Marked as FrI-1, FrI-2, FrI-3, FrI-4, FrI-5.
[0077] Dissolve the concentrated FrI-4 with a small amount of methanol for separation on silica gel H. The eluent is a mixed ...
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