A method for separating trace alkaloid monomers from total alkaloids of Cortex Morus alba

A technology of biological total alkaloids and Morus alba, applied in medical preparations containing active ingredients, plant/algae/fungus/moss ingredients, pharmaceutical formulas, etc., can solve rare and other problems

Active Publication Date: 2018-02-27
HEFEI HUAFANG PHARMA SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are more and more reports on the hypoglycemic research of the total alkaloids of Cortex Mori, especially 1-deoxynojirimycin (DNJ), but there are few antidiabetic drugs of the total alkaloids of Cortex Mori.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The preparation of embodiment 1 Morus alba alkaloid monomer

[0021] (1), derivatization reaction:

[0022] Take an appropriate amount of the total alkaloids of Cortex Morus alba, dissolve in 10 times the amount of methanol, concentrate the filtrate to dryness under reduced pressure, and add 6 times the amount (the total alkaloids of Cortex Morus alba) of sodium carbonate-bicarbonate with a pH of 9.0 Sodium buffer solution and tetrahydrofuran 1:1 mixed solution were dissolved, slowly added 3 times the amount of 9-fluorenylmethoxyacyl chloride (Fmol-Cl) reagent, stirred for 10 hours, added 5 times the amount of water to dilute, sequentially extracted with petroleum ether, and used ring Extract with hexane, discard the organic layer, extract the aqueous layer with ethyl acetate, recover the organic solvent under reduced pressure to obtain derivatives, and set aside.

[0023] (2), column separation:

[0024] Take the above-mentioned derivatives—put them on a 100-200 mesh...

Embodiment 2

[0032] The preparation of embodiment 2 Alba Morus alba alkaloid monomer

[0033] (1), derivatization reaction:

[0034] Take an appropriate amount of the total alkaloids of Cortex Morus alba, dissolve in 1 times the amount of methanol, concentrate the filtrate to dryness under reduced pressure, add 4 times the amount (the total alkaloids of Cortex Morus alba) with pH 9.0 of sodium carbonate-bicarbonate Sodium buffer solution and tetrahydrofuran 1:1 mixed solution dissolved, slowly added 0.5 times the amount of 9-fluorenylmethoxyacyl chloride (Fmol-Cl), stirred for 2 hours, added 10 times the amount of water to dilute, followed by extraction with petroleum ether, and cyclohexane Extract with alkane, discard the organic layer, extract the aqueous layer with ethyl acetate, recover the organic solvent under reduced pressure to obtain derivatives, and set aside.

[0035] (2), column separation:

[0036] Take the above-mentioned derivatives—put them on a 100-200 mesh silica gel co...

Embodiment 3

[0044] The preparation of embodiment 3 Morus alba alkaloid monomer

[0045] (1), derivatization reaction:

[0046] Take an appropriate amount of the total alkaloids of Cortex Morus alba, dissolve in 20 times the amount of methanol, concentrate the filtrate to dryness under reduced pressure, and add 8 times the amount (the total alkaloids of Cortex Morus alba) of sodium carbonate-bicarbonate with a pH of 9.0 Sodium buffer solution and tetrahydrofuran 1:1 mixed solution were dissolved, slowly added 5 times the amount of 9-fluorenylmethoxyacyl chloride (Fmol-Cl), stirred for 2 hours, added 20 times the amount of water to dilute, sequentially extracted with petroleum ether, and used cyclohexane Extract with alkane, discard the organic layer, extract the aqueous layer with ethyl acetate, recover the organic solvent under reduced pressure to obtain derivatives, and set aside.

[0047] (2), column separation:

[0048] Take the above-mentioned derivatives—put them on a 100-200 mesh ...

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PUM

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Abstract

The invention relates to a technical method for separating monomers with hypoglycemic alkaloid activity such as fagopyrin, 1,4-dideoxy-1,4-imino-d-arabinitol and 1-deoxynojirimycin from white mulberry root-bark total alkaloid. The method comprises the following steps: by using the self-extracted white mulberry root-bark total alkaloid as a primary material, re-dissolving through methyl alcohol to remove most of DNJ (1-deoxynojirimycin); concentrating eluent, then performing derivatization reaction, performing column chromatography through a silica gel column, obtaining multiple active alkaloid monomers through column elution, and finally, dissociating derivatized groups to obtain the alkaloid monomers. The content of the obtained monomers exceeds 95.0 percent, and the monomers can be used as standard reference materials or other materials.

Description

technical field [0001] The invention relates to a technical method for extracting and separating buckwheatine, 1,4-dideoxy-1,4-imino-d-arabinitol, 1-deoxynojirimycin and other alkaloid active monomers from the total alkaloids of Morus alba and technical points. Background technique [0002] The drugs currently on the market for the treatment of diabetes are mainly sulfonylureas, biguanides and α-glucosidase inhibitors. However, sulfonylureas are likely to cause persistent hypoglycemia, and biguanides can cause severe gastrointestinal reactions and liver and kidney damage, while α-glucosidase inhibitors have fewer adverse reactions except for increased intra-abdominal gas. It has been widely used to reduce postprandial hyperglycemia. At present, the α-glucosidase inhibitor drugs clinically used to treat diabetes include Baitangping, Beixin and Morus alba and related drugs in domestic traditional Chinese medicine. Domestic hypoglycemic Chinese patent medicines are mainly ma...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D211/46C07D207/12A61K36/605
CPCA61K36/605C07D207/12C07D211/46
Inventor 张亮亮杨贤龙何勇
Owner HEFEI HUAFANG PHARMA SCI & TECH
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