Preparation method for preparing sodium copper chlorophyllin from gingko leaves

A technology of copper chlorophyllin sodium salt and chlorophyllin cupric acid, which is applied in the field of preparing copper chlorophyllin sodium salt from ginkgo leaves, can solve the problems of high cost and low purity, achieve stable quality, high purity, and reduce production costs

Active Publication Date: 2015-06-24
ZHEJIANG DELEKANG FOOD CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a low-cost, high-purity, convenient and quick method for preparing copper chlorophyllin so

Method used

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  • Preparation method for preparing sodium copper chlorophyllin from gingko leaves
  • Preparation method for preparing sodium copper chlorophyllin from gingko leaves
  • Preparation method for preparing sodium copper chlorophyllin from gingko leaves

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042]Take 0.5Kg of dried ginkgo leaves, analyze by liquid phase and contain 0.3% pheophytin, crush them, add 1.5L of No. 6 solvent oil and soak at 30°C for 1 hour, filter, and rinse the filter residue with 1L of No. 6 solvent oil; the extract Contain 1.35g of pheophytin by liquid phase analysis; concentrate the extract to 20% of the mass of Ginkgo biloba leaves, add 200mL of 80% isopropanol, 200mL of No. 6 solvent oil, shake well, transfer to a brown 1000mL jar, place In a water bath at 60°C, add 32mL of 30% (w / w) liquid caustic soda, 16mL of 20% (w / w) copper sulfate aqueous solution, shake well and let stand to saponify 0.5% of the water; Stand in the separatory funnel for stratification; discard the middle layer and the upper layer, transfer the lower layer to a continuous liquid-liquid extractor, and use No. 6 solvent oil to extract the oil-soluble impurities until the effluent of No. 6 solvent oil is light in color; remove the lower layer of soap Add 400mL of No. 6 solven...

Embodiment 2

[0045] Take 0.5Kg of dried Ginkgo biloba leaves, analyze by liquid phase and contain 0.3% pheophytin, pulverize, add 1.5L of 60% ethanol, 1.5L of No. 6 solvent oil, stir and extract at 45°C for 4 hours, let it stand for stratification, and replenish the lower layer. Add 1.5L of No. 6 solvent oil, stir for 30 minutes, and then let stand to separate layers; combine the No. 6 solvent oil phase to obtain the pheophytin extract; this extract contains 1.41g of pheophytin through liquid phase analysis; concentrate the extract to 45% of the mass of ginkgo leaves, add 200mL of 90% isopropanol, 200mL of No. 6 mineral spirits, shake well, transfer to a brown 1000mL wide-mouth bottle, put it in a water bath at 50°C, and add 32mL of 30% (w / w) liquid caustic soda , 16 mL of 20% (w / w) copper sulfate aqueous solution, shake well and let stand to saponify 2 hours of water; add 400 mL of water to the soap solution, transfer it into a well-protected separatory funnel and let it stand for stratifi...

Embodiment 3

[0048] Take 0.5Kg of dried Ginkgo biloba leaves, analyze by liquid phase and contain 0.3% pheophytin, crush them, add 1.5L of No. 6 solvent oil, let stand and soak at 60°C for 6 hours, filter, and wash the filter residue with 1L of No. 6 solvent oil; The extract was analyzed by liquid phase to contain 1.37g of pheophytin; concentrate the extract to dryness, add 100% isopropanol 100mL, No. 6 solvent oil 200mL, shake well, transfer to a brown 1000mL wide-mouth bottle, put in a 40°C water bath Add 32mL of 30% (w / w) liquid caustic soda, 16mL of 20% (w / w) copper sulfate aqueous solution, shake well and let stand for saponification for 20 hours; add 200mL of water to the soap solution and transfer it into a well-protected separatory funnel Leave to stand for stratification; discard the middle layer and the upper layer, transfer the lower layer to a continuous liquid-liquid extractor, and extract the oil-soluble impurities with No. 6 solvent oil until the effluent of No. 6 solvent oil...

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Abstract

The invention relates to a preparation method for preparing sodium copper chlorophyllin from gingko leaves. The preparation method comprises the following main steps: performing extraction and concentration; performing saponification and copper substitution; extracting and removing impurities from the No.6 solvent oil under an alkaline soap solution; removing ginkgolic acid; and forming a salt. According to the preparation method, before, during or after leaching gingko flavones by using a polar solvent, a non-polar solvent is used as a leaching solvent to perform leaching on chlorophyll and other oil-soluble substances; a mixed solvent is adopted as a dissolvent to perform saponification, so that the existence and generation of a deposit in the soap solution are effectively avoided, and then the reaction can be quickly and completely performed; and sodium copper chlorophyllin is prepared by a method comprising the processes of alkaline saponification and copper substitution which are performed simultaneously, so that esterification and deterioration of chlorophyll copper acid during acidic copper substitution are avoided. According to the product obtained by the preparation method provided by the invention, the E1%1cm(405nm+/-nm) is more than 900, the absorbance ratio is equal to 3.2-3.6, the complex copper content is more than 6%, the nitrogen content is more than 5.5%, and the ginkgolic acid content is less than 50ppm.

Description

technical field [0001] The invention relates to the technical field of plant extraction, in particular to a method for preparing sodium copper chlorophyllin quickly from ginkgo leaves with low ginkgolic acid content. Background technique [0002] Our country is rich in Ginkgo biloba resources, but there are very few enterprises that use Ginkgo biloba for comprehensive development. Most of them only use it to extract Ginkgo biloba extract, and few companies comprehensively utilize other substances rich in Ginkgo biloba. [0003] The sodium copper chlorophyllin salt sold on the market generally has a complexed copper content of <4.5%. According to the theoretical complexed copper content of 9%, its chlorophyll content is <50%, and the rest is organic acid sodium salt. Commercially available sodium copper chlorophyllin is mostly extracted from silkworm excrement. However, since the chlorophyll in clamworm needs to be acidified for copper generation, and the chlorophyll is...

Claims

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Application Information

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IPC IPC(8): C07D487/22C07C33/02C07C29/76
CPCC07D487/22
Inventor 崔升官童舜火张锦红柯炜祥
Owner ZHEJIANG DELEKANG FOOD CO LTD
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