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Protosappanin B preparation method

A technology of hematoxylin and resin, which is applied in the chemical field, can solve the problem of not disclosing the high content of prohematoxylin, and achieve the effect of low cost

Inactive Publication Date: 2018-07-27
黄榜昇
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The prior art has not disclosed that the bark of the wood butterfly contains higher levels of prohematoxylin A, B, C

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0059] Embodiment 1: the preparation method of protohematoxylin A

[0060] A method for preparing prohematoxylin A, comprising the steps of:

[0061]Step S1, crushing the dry bark of the wood butterfly, and extracting with 85% ethanol aqueous solution under heat reflux for 3 times, each time for 2 hours, with a solid-liquid ratio of 1:20; combining the extracts obtained 3 times, filtering, Collect the filtrate, concentrate the filtrate to no alcohol smell as the sample solution of the macroporous resin;

[0062] Step S2, load the obtained sample solution on the AB-8 macroporous resin column, the diameter-to-height ratio of the resin is 1:10, and the resin mixed with the sample accounts for 1 / 10 of the total resin, and the column is wet packed, and the resin is mixed with the sample ; Use 35%, 55%, and 75% ethanol to elute 8, 8, and 5 BV respectively at a flow rate of 12 BV / h, collect 4-5 BV eluents of 75% ethanol, concentrate and dry to obtain crude prohematoxylin;

[0063] ...

Embodiment 2

[0066] Embodiment 2: the preparation method of prohematoxylin B

[0067] A method for preparing prohematoxylin B, comprising the steps of:

[0068] Step S1, crushing the dry bark of the wood butterfly, and extracting with 85% ethanol aqueous solution under heat reflux for 3 times, each time for 2 hours, with a solid-liquid ratio of 1:20; combining the extracts obtained 3 times, filtering, Collect the filtrate, concentrate the filtrate to no alcohol smell as the sample solution of the macroporous resin;

[0069] Step S2, load the obtained sample solution on the AB-8 macroporous resin column, the diameter-to-height ratio of the resin is 1:10, and the resin mixed with the sample accounts for 1 / 10 of the total resin, and the column is wet packed, and the resin is mixed with the sample ; Use 35%, 55%, and 75% ethanol to elute 8, 8, and 5 BV respectively at a flow rate of 12 BV / h, collect 4-5 BV eluents of 75% ethanol, concentrate and dry to obtain crude prohematoxylin;

[0070] S...

Embodiment 3

[0073] Embodiment 3: the preparation method of prohematoxylin C

[0074] A method for preparing prohematoxylin C, comprising the steps of:

[0075] Step S1, crushing the dry bark of the wood butterfly, and extracting with 85% ethanol aqueous solution under heat reflux for 3 times, each time for 2 hours, with a solid-liquid ratio of 1:20; combining the extracts obtained 3 times, filtering, Collect the filtrate, concentrate the filtrate to no alcohol smell as the sample solution of the macroporous resin;

[0076] Step S2, load the obtained sample solution on the AB-8 macroporous resin column, the diameter-to-height ratio of the resin is 1:10, and the resin mixed with the sample accounts for 1 / 10 of the total resin, and the column is wet packed, and the resin is mixed with the sample ; Use 35%, 55%, and 75% ethanol to elute 8, 8, and 5 BV respectively at a flow rate of 12 BV / h, collect 4-5 BV eluents of 75% ethanol, concentrate and dry to obtain crude prohematoxylin;

[0077] S...

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Abstract

The invention discloses a protosappanin B preparation method. The method includes steps: step S1, grinding dried bark of oroxylum indicum, extracting with 75%-95% ethanol, filtering and concentratinguntil alcoholic smell disappears, and taking as loading buffer; step S2, loading the loading buffer to a macroporous resin column, sequentially adopting 35%, 55% and 75% ethanol to elute by 8, 8 and 5BV by a flow rate of 12BV / h, collecting 4-5BV elution liquid of 75% ethanol, and concentrating and drying to obtain a crude protosappanin product; step S3, taking ethyl acetate, n-butyl alcohol, tetrahydrofuran and water in a volume ratio of 20:3.5:1.5:10 to form a solvent system, wherein an upper phase is taken as a stationary phase, and a lower phase is taken as a mobile phase; fully pumping thestationary phase into a pipeline, pumping the mobile phase by a forward rotating velocity of 850r / min, and injecting the crude protosappanin product dissolved with the lower phase into a sample injection ring when the mobile phase flows out of a mainframe outlet; by the detection wavelength of 245nm, collecting elution liquid corresponding to protosappanin B according to a chromatogram, concentrating and drying.

Description

technical field [0001] The invention belongs to the field of chemistry and relates to a method for preparing prohematoxylin A, B and C. Background technique [0002] Protohematoxylin A, B, and C are the first three simple biphenyl compounds found in hematoxylin, and their chemical structures are as follows. [0003] [0004] Studies have shown that protohematoxylin A, B, and C have various pharmacological activities and have broad prospects (reference: Study on the radiosensitization effect of protohematoxylin A on gastric cancer SGC-7901 cell line, Journal of Practical Oncology, Issue 6, 2017; protohematoxylin A Experimental Study on Regulating the Maturation and Functional State of Dendritic Cells, Journal of Cardiovascular Rehabilitation Medicine, Issue 4, 2017; Research on the Inhibitory Effect of Protohematoxylin B on Tumor Cells BTT T24Hela and SW480, China Drugs and Clinics, Issue 8, 2015; Protohematoxylin Inhibitory effect of B on the proliferation of bladder can...

Claims

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Application Information

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IPC IPC(8): C07D313/20
CPCC07D313/20
Inventor 黄榜昇
Owner 黄榜昇
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