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Method for preparing 4-O-methyl hematoxylin through separation

A technology of hematoxylin and methyl, applied in the field of separation and preparation of 4-O-methyl hematoxylin, can solve the problems of cumbersome methods, unsuitable for industrial production, and low repeatability, achieve low separation cost, overcome long separation cycle, repeatability, etc. strong effect

Pending Publication Date: 2022-06-28
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, most of the methods for separating 4-O-methylhematoxylin from hematoxylin require complex extraction, multi-stage extraction, and multiple silica gel column chromatography separations. The methods are cumbersome and have low repeatability, and are not suitable for industrial production.

Method used

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  • Method for preparing 4-O-methyl hematoxylin through separation
  • Method for preparing 4-O-methyl hematoxylin through separation
  • Method for preparing 4-O-methyl hematoxylin through separation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] A method for separating and preparing 4-O-methylhematoxylin is carried out according to the following steps:

[0036] (1) Extraction of hematoxylin crude extract

[0037] Weigh 1 kg of hematoxylin decoction pieces in the extraction tank, extract 2 times with 5L 75% ethanol under reflux, 2 hours each time, cool and filter, the alcohol extracts are combined and concentrated under reduced pressure under a vacuum rotary evaporator at 50 °C to obtain 97 g of alcohol extract ;

[0038] (2) Preparation of hematoxylin ethyl acetate extract

[0039] After fully dissolving the alcohol extract with water at a ratio of 1:2, extract it with an equal volume (2000 mL) of petroleum ether for 3 times to remove the small polar part in the hematoxylin, remove the phase and then use an equal volume (2000 mL) of ethyl acetate. Ester extraction was performed twice, the ethyl acetate extracts were combined and concentrated under reduced pressure under a vacuum rotary evaporator at 50°C to o...

Embodiment 2

[0047] (1) Extraction of hematoxylin crude extract

[0048] Weigh 1 kg of hematoxylin decoction pieces, and extract 2 times with 5 L of 95% ethanol under reflux for 2 h each time. The extracts are combined and concentrated under reduced pressure under a vacuum rotary evaporator at 50 °C to obtain 60 g of alcohol extract;

[0049] (2) Preparation of hematoxylin ethyl acetate extract

[0050] After fully dissolving the alcohol extract described in the step (1) according to the water with a material-to-liquid ratio of 1:2, first extract it 3 times with an equal volume (2000 mL) of petroleum ether, remove the small polar part in the hematoxylin, remove the phase, and then extract it again. It was extracted twice with equal volume (2000 mL) of ethyl acetate, and the ethyl acetate extract was taken and concentrated under reduced pressure under a vacuum rotary evaporator at 50° C. to obtain 12 g of ethyl acetate extract.

[0051] (3) Preparation of hematoxylin samples

[0052] Weig...

Embodiment 3

[0057] Based on Example 1, the injection concentration in the preparative high performance liquid chromatography was investigated, as shown below, and other steps refer to Example 1.

[0058] The hematoxylin sample described in step (3) was dissolved in methanol. A preparative column with octadecylsilane-bonded silica gel as the filler was selected, the model is SHIM-PACK, PRC-ODS (H) (20mm×250mm, 15μm), and acetonitrile (A)-pure water (B) (12: 88, v / v) is the mobile phase, isocratic elution, the injection concentration is 100mg / mL, the injection volume is 1mL, the flow rate is 1.0mL / min, the column temperature is room temperature, the detection wavelength is 285nm, and the liquid chromatogram is collected and prepared Elution fractions with retention times of 40.2-42 min, see Figure 8 . The preparative liquid phase separation effect under this condition is acceptable, but the solvent effect is large due to the large injection volume. The purity of the target fraction was ...

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Abstract

The invention discloses a method for separating and preparing 4-O-methyl hematoxylin, which combines a column chromatography technology and a preparative high performance liquid chromatography technology, and can separate and obtain 4-O-methyl hematoxylin with the purity of more than 95.0% from hematoxylon. The 4-O-methyl hematoxylin prepared through separation is high in purity, large in preparation amount, rapid, efficient and suitable for batch production of the 4-O-methyl hematoxylin.

Description

technical field [0001] The invention relates to the field of preparation of active ingredients of traditional Chinese medicines, in particular to a method for separating and preparing 4-O-methyl hematoxylin. Background technique [0002] Hematoxylin is the dried heartwood of the legume Caesalpinia sappan L. It is native to India, Myanmar and other Southeast Asian regions. In my country, it is mainly distributed in Guangdong, Guangxi, Yunnan and other places. The main planting area is mainly Guangxi. Studies have shown that hematoxylin contains a variety of chemical components, including dibezoxocin derivatives, brazilianes, homoisoflavonoids, and chalcones. Among them, the high isoflavones have shown good biological activities in anti-inflammatory, antifungal, neuroprotective, hepatocyte protection, inhibition of melanocyte growth and anti-angiogenesis due to their structural properties. However, so far, from There are only more than 100 kinds of natural high isoflavone com...

Claims

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Application Information

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IPC IPC(8): C07D311/94
CPCC07D311/94C07B2200/07
Inventor 张慧吴亚梦颜继忠
Owner ZHEJIANG UNIV OF TECH
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