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Method for preparing indigo blue and indirubin from fresh Baphicacanthus cusia leaves

A technology of indirubin and fresh leaves is applied in the field of indirubin and indigo preparation, which can solve the problems of low yield and the like, and achieve the effect of good adsorption effect and simplified technological process.

Active Publication Date: 2021-05-21
哈工大机器人南昌智能制造研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Mix wood ash, lime and bran into the indigo, add water to mix, heat to 30-40°C, and expose to the air to become blue insoluble indigo with low yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Weigh 1kg of fresh leaves of Ma Lan, put them in tap water at 30°C with a pH of 5.5, wherein the volume of water is 30 times the mass of the fresh leaves, aerate and stir once for 1 hour, soak for 48 hours, filter through a sieve to remove the leaf residue, and add alkali to adjust The pH of the soaking solution was adjusted to 10.5, and the soaking solution was heated to 60 degrees, while aerating and stirring for 1 h, adding 8% pretreated D3520 macroporous resin to the soaking solution, stirring and beating for 40 min. D3520 resin was packed into a 500 x 10 mm glass column. First wash water-soluble impurities with water, then wash fat-soluble impurities with 4BV of 50% ethanol, and finally dissociate with 6BV of 100% ethanol at a flow rate of 3BV / h, collect the dissociated liquid, and rotate to concentrate to obtain 58.25g of crude indigo indirubin. The contents of indigo and indirubin detected by RP-HPLC were 16.13g / kg and 5.81g / kg respectively, and the purity of ind...

Embodiment 2

[0021] Weigh 1 kg of fresh leaves and place them in tap water with a pH of 5.5 at 30°C, where the water quality is 30 times that of the fresh leaves. Aerate for 1 hour and stir once. After soaking for 48 hours, filter through a sieve to remove the leaf residue. Add NaOH to the soaking solution to adjust the pH of the filtrate to 10.5. Heat the soaking solution to 60 degrees. After stirring and beating the indigo for 40min, the precipitate was collected by filtration, the filtrate was re-filtered and recovered, the precipitate was mixed with water, and the water was removed to remove impurities to obtain 183.14 g of indigo paste. The yields of the product indigo indirubin detected by RP-HPLC were 15.02g / kg and 5.29g / kg, respectively.

Embodiment 3

[0023] Producing Indigo Indirubin from Indigo Plaster by Ultrasound-Assisted Method

[0024] The indigo paste prepared by the method in Example 2 was added with 4 times of ethanol and stirred with 100W ultrasonic treatment for 30min, filtered, and the filter residue was extracted twice with ethanol to combine the three filtrates, and the ethanol solvent was concentrated and recovered by rotary evaporation. After reaching a certain concentration, the same amount of ethanol was added. of distilled water. After concentrating and recovering 1 / 2 of the water, cooling and filtering, the filter residue is 55.32 g of crude indigo indirubin. The content of indigo and indirubin detected by RP-HPLC method is 24.75% and 10.28% respectively.

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Abstract

The invention discloses a method for preparing indigo blue and indirubin from fresh baphicacanthus cusia leaves. The method comprises the following steps: (1) soaking and fermenting the fresh baphicacanthus cusia leaves; (2) synthesizing indigo; (3) extracting indigo; (4) purifying indigo blue indirubin; and (5) separating and purifying by a chromatographic column. According to the invention, lime is not added to settle, but is directly replaced by adsorption resin. The adsorption effect is better than that of calcium carbonate; the process flow is simplified, calcium carbonate impurity removal is omitted, and column elution purification can be directly performed; the resin can be recycled, and the yield and purity of obtained indirubin and indigo blue are higher than those of indirubin and indigo blue obtained by a conventional process.

Description

technical field [0001] The invention belongs to the field of natural product extraction, and in particular relates to a method for preparing indigo and indirubin by adopting fresh horse blue leaves. Background technique [0002] Baphicacanthus cusia Brem is a perennial herb belonging to the genus Baphicacanthus cusia, which is widely distributed in Southwest my country, South China and East China. Malanga root, stem and leaves can be used as medicine. Its roots and stems are used as Radix isatidis, and the dried leaves are used as Daqingye. The raw materials for the preparation of indirubin mainly include "blue" plants such as horse indigo, isatis indigo and polygonum indigo, among which indirubin has the highest content in fresh horse blue leaves, and the stems and leaves of horse blue contain a large amount of indigo precursor substances - indigo Indole glycosides or free indoxyl, the finished product indigo processed from the stems and leaves of Ma blue, has high indiru...

Claims

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Application Information

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IPC IPC(8): C09B7/02
CPCC09B7/02
Inventor 赵亮刘兆宇
Owner 哈工大机器人南昌智能制造研究院
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