Preparation method of eugeniin

A clove, extraction technology, applied in the preparation field of extracting syringin from plants, can solve the problems such as no application of high-purity syringin preparation process report, and achieve the effects of large-scale production operation, less pollution, and less energy consumption

Inactive Publication Date: 2012-01-25
SUZHOU PAITENG BIOLOGICAL MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In the prior art, there is no report on the preparation process applicable to the industrialized large-scale production of high-purity syringin

Method used

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  • Preparation method of eugeniin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Take 10Kg of clove leaves, add 80Kg of water, put it into a microwave extraction device for microwave extraction, extraction power 400W, extract once, 3 minutes, collect the extract, filter, filter the filtrate through an activated carbon column to absorb impurities, and collect the next column liquid , adsorbed by D102 macroporous adsorption resin column, eluted with 10% ethanol, collected 3 times the column volume eluate, concentrated, added ethanol to make the alcohol content reach 65%, refrigerated for 24 hours, filtered, collected filter residue, and dried , Pulverize to obtain 59.5g of syringin, detected by HPLC, the purity is 94.2%, UV, IR, MS, 2 HNMR, 13 The data characterizing its physical properties such as CNMR are consistent with the prior art.

Embodiment 2

[0026] Take 10Kg of clove leaves, add 120Kg of water, put it into a microwave extraction device for microwave extraction, extraction power 600W, extract 3 times, 8 minutes each time, collect the extract, filter, and the filtrate is adsorbed by an activated carbon column to remove impurities and collected. The column liquid is adsorbed by the AB-8 macroporous adsorption resin column, eluted with 30% ethanol, collected 8 times the column volume eluate, concentrated, added ethanol to make the alcohol content reach 65%, refrigerated for 24 hours, filtered, The filter residue was collected, dried and pulverized to obtain 68.3 g of syringin, which was detected by HPLC with a purity of 92.9%, UV, IR, MS, 2 HNMR, 13 The data characterizing its physical properties such as CNMR are consistent with the prior art.

Embodiment 3

[0028] Take 10Kg of clove leaves, add 100Kg of water, put it into a microwave extraction device for microwave extraction, extraction power 500W, extraction 2 times, 6 minutes each time, collect the extract, filter, and the filtrate is adsorbed by activated carbon column to remove impurities. Collect the lower column liquid, absorb it through a D101 macroporous adsorption resin column, elute with 20% ethanol, collect 5 times the column volume eluate, concentrate, add ethanol to make the alcohol content reach 65%, refrigerate for 24 hours, filter, The filter residue was collected, dried and pulverized to obtain 63.5 g of syringin, which was detected by HPLC with a purity of 96.3%, UV, IR, MS, 2 HNMR, 13 The data characterizing its physical properties such as CNMR are consistent with the prior art.

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Abstract

The invention relates to a preparation method of eugeniin, which is easy and convenient to operate and has small pollution and low energy consumption. The method comprises the following process steps of: adding clove leaves into water; putting into a microwave extraction device for undergoing microwave extraction at the extraction power 400-600W for 1-3 times every time for 3-8 minutes; collecting an extraction liquid; filtering; making a filtrate pass through an active carbon column for adsorbing and removing impurities; collecting a column unloading liquid; adsorbing with a macroporous absorption resin column; eluting with ethanol; collecting an eluent; concentrating; adding ethanol till the alcohol content is up to 65 percent; refrigerating for 24 hours; filtering; collecting filter residues; and drying and smashing. Due to the adoption of the method for preparing eugeniin, the product purity is high and industrial amplification is easy to realize.

Description

technical field [0001] The invention relates to a preparation method of syringin, in particular to a preparation method of extracting syringin from plants. Background technique [0002] Eugeniin (Eugeniin), molecular formula: C 41 h 30 o 26 , Molecular weight: 938.672, CAS registration number: 58970-75-5, mainly found in various plants of Myrtaceae, Cornaceae, Willowaceae, and Faguceae. of which myrtaceae cloves Eugenia caryophllata Thunb. is abundant in leaves, and its molecular formula is as follows. [0003] [0004] Modern studies have shown that syringin has various functions such as anti-virus and anti-tumor, and it is also used as a raw material for the synthesis of other active derivatives. [0005] myrtle clove Eugenia caryophllata The dried flower buds of Thunb. are used as a traditional Chinese medicine clove, which warms the middle and lowers adverse events, nourishes the kidney and supports yang. For spleen and stomach deficiency and cold, hiccups an...

Claims

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Application Information

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IPC IPC(8): C07H13/08C07H1/08
Inventor 王峰王琳张发成
Owner SUZHOU PAITENG BIOLOGICAL MEDICAL TECH
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