CN110372767B

CN110372767B - Method for extracting and separating white rhododendron from rhododendron roseum leaves

Info

Publication number: CN110372767B
Application number: CN201910269729.1A
Authority: CN
Inventors: 梁俊玉; 逯佩玉; 邵亚洲; 徐婕; 杨盈盈; 王俊龙; 孔维宝
Original assignee: Northwest Normal University
Current assignee: Northwest Normal University
Priority date: 2019-04-04
Filing date: 2019-04-04
Publication date: 2023-03-24
Anticipated expiration: 2039-04-04
Also published as: CN110372767A

Abstract

The invention provides a method for extracting and separating white azalea from rhododendron leaf, which is characterized in that rhododendron leaf powder is taken as a raw material and added into petroleum ether for reflux; air drying the residue, adding into anhydrous ethanol, reflux extracting for 3 times, and mixing extractive solutions; concentrating the extractive solution until no alcohol smell exists, adding water for dissolving, adding into polyamide column, and eluting with distilled water; collecting water eluent, concentrating the water eluent into thick paste with the density of 1.05 to 1.15, adding absolute ethyl alcohol, and heating to dissolve the thick paste; filtering while hot, removing insoluble substances, cooling the filtrate, and crystallizing to obtain light yellow powder; adding anhydrous ethanol into the light yellow powder, heating to dissolve, filtering while hot, removing insoluble substances, and cooling the filtrate for recrystallization to obtain colorless needle crystal product. And identifying the extracted white farrerol to determine that the white farrerol is white farrerol. And the yield of the rhododendron is 3.5-4.5%, and the purity is 95-98%. The method has the advantages of simple process, no toxicity, environmental protection and suitability for industrial production.

Description

Method for extracting and separating rhododendron white from rhododendron leaf

Technical Field

The invention relates to a method for extracting and separating white rhododendron from a long-noded rhododendron leaf, belonging to the technical field of extraction and separation of effective active ingredients of plants.

Background

White azalea, english name: rhododendron; CAS number: 497-78-9; the molecular formula is as follows: c ₁₆ H ₂₄ O ₇ (ii) a Molecular weight: 328.35756. the structural formula is as follows:

the white rhododendron is reported to have analgesic and anti-inflammatory effects in the literature. Few documents are reported on the extraction and separation of the rhododendron in white, and the only report is that in rhododendron pulchrum: (A)Rhododendron aureum) The content of the white rhododendron separated from the leaves is 0.48 percent, the separation method is complex, the dosage of the organic solvent is large, and the content is not high.

Long Shu Juan (Rhododendron przewalskii Maxim.) is a plant of Ericaceae, and the Tibetan medicine is called Damma, which is mainly distributed in Shaanxi, gansu, qinghai and Sichuan provinces in China and has large reserves. Has effects in clearing lung-heat, purging pathogenic fire, relieving cough, eliminating phlegm, and treating cough, asthma, senile chronic bronchitis, hypertension, and coronary heart disease. At present, no report of extracting and separating the white rhododendron by using the rhododendron is available.

Disclosure of Invention

The invention aims to provide a method for extracting and separating white rhododendron from rhododendron septemlobum leaves.

1. Extraction and separation of rhododendron

(1) Adding the rhododendron flofolium powder into petroleum ether for refluxing; air drying the residue, extracting with anhydrous ethanol under reflux for 3 times, and mixing extractive solutions.

In the petroleum ether reflux, the ratio of the longshu rhododendron leaf powder to the petroleum ether is 0.1-0.3 g/ml, the reflux temperature is 65-90 ℃, and the reflux time is 1-2h; putting the medicine residue in ethanol, wherein the ratio of the medicine residue to the feed liquid of the ethanol is 0.05-0.2g/ml, the reflux extraction temperature is 70-80 ℃, and the reflux time is 40-45min each time.

(2) Concentrating the extractive solution until no alcohol smell exists, adding water for dissolving, adding into polyamide column for adsorbing impurities, and eluting with distilled water; the dosage of the polyamide is 0.25 to 1 time of the mass of the folium Rhododendri Simsii; the water consumption for elution is 5 to 15 times of the mass of the polyamide.

(3) Collecting water eluent, concentrating the water eluent into thick paste with the density of 1.05 to 1.15, adding absolute ethyl alcohol, and heating to dissolve the thick paste; filtering while hot, discarding insoluble substances, cooling the filtrate, and crystallizing to obtain light yellow powder.

(4) Adding anhydrous ethanol into the yellowish powder, heating for dissolving, filtering while hot, removing insoluble substances, cooling the filtrate, and recrystallizing to obtain colorless needle crystal, i.e. white farrerol.

The yield of the rhododendron is 3.5-4.5%, and the purity is 95-98%.

2. Identification of rhododendron albopicolide

The obtained colorless needle crystal is analyzed and identified by methods such as mass spectrum, nuclear magnetic resonance hydrogen spectrum, carbon spectrum, X-ray diffraction and the like, and is white farrerol.

In summary, compared with the prior art, the invention has the following beneficial effects:

1. the raw material of the Longshu rhododendron is abundant in domestic resources, wide in distribution, easy to obtain, and high in content of white azalea, so that the difficulty and the cost of raw material collection can be greatly reduced; meanwhile, the used plant material, namely the longshu cuckoo has rich resources, and the used parts are leaves, so that the ecological environment is not damaged, and the sustainable development is facilitated;

2. the invention adopts petroleum ether to carry out thermal reflux on the crushed raw materials to remove pigment and fat-soluble impurities, so that the impurities in the alcohol extract are reduced, the amount of a crude extract is increased when the crude extract passes through a polyamide column, and the efficiency is improved;

3. the method has the advantages of simple process flow, low cost and less resource consumption; the obtained white rhododendron has high yield and high purity;

4. the invention uses less reagent types, is cheap, easy to obtain, nontoxic and harmless to the environment and workers. And after elution, the polyamide can be reused after regeneration.

Drawings

FIG. 1 is a high resolution mass spectrum of the extracted product of the present invention.

FIG. 2 is a nuclear magnetic resonance hydrogen spectrum of the extracted product of the present invention.

FIG. 3 is a carbon spectrum of the product of the present invention.

FIG. 4 is an X-ray diffraction pattern of the extracted product of the present invention.

Detailed Description

The method for extracting and separating rhododendron white from rhododendron septemlobum leaves of the present invention is further described in the following embodiments.

Example 1

(1) Pulverizing folium Rhododendri Simsii, and sieving with 40 mesh sieve. Weighing 100g of rhododendron flosum leaf powder, adding 500ml of petroleum ether, and refluxing at 70 ℃ for 2h; air drying the residue, adding 1000mL of anhydrous ethanol, extracting at 80 deg.C under reflux for 3 times, each for 45min, and mixing extractive solutions;

(2) Concentrating the extractive solution until no alcohol smell exists, adding 300ml water for dissolving, adding into 200g polyamide column, and eluting with 2000ml distilled water;

(3) Collecting water eluate, concentrating to obtain soft extract with density of 1.05, adding 150ml anhydrous ethanol, and heating for dissolving; filtering while hot, removing insoluble substances, cooling the filtrate, and crystallizing to obtain light yellow powder;

(4) Adding 45ml of absolute ethyl alcohol into the pale yellow powder, heating and dissolving, filtering while hot, removing insoluble substances, cooling the filtrate, and recrystallizing to obtain 3.8g of colorless needle crystal white azalea with the purity of 97%.

Example 2

(1) Pulverizing folium Rhododendri Simsii, and sieving with 50 mesh sieve. Weighing 100g of rhododendron leaf powder, adding 700ml of petroleum ether, and refluxing at 80 ℃ for 1h; air drying the residue, adding anhydrous ethanol 800mL, and extracting at 75 deg.C under reflux for 45min for 3 times; mixing extractive solutions

(2) Concentrating the extractive solution until no alcohol smell exists, adding 250ml of water for dissolving, adding into 100g of polyamide column, and eluting with 1500ml of distilled water;

(3) Collecting water eluate, concentrating to obtain soft extract with density of 1.08, adding 200ml anhydrous ethanol, and heating for dissolving; filtering while hot, removing insoluble substances, cooling the filtrate, and crystallizing to obtain light yellow powder;

(4) Adding 50ml of absolute ethyl alcohol into the light yellow powder, heating for dissolving, filtering while hot, removing insoluble substances, cooling the filtrate, and recrystallizing to obtain 4.2g of colorless needle crystal white azaleatin with the purity of 96%.

Example 3

(1) Pulverizing folium Rhododendri Simsii, and sieving with 60 mesh sieve. Weighing 100g of rhododendron leaf powder, adding 800ml of petroleum ether, and refluxing at 65 ℃ for 1.5h; air drying the residue, adding 1200mL of anhydrous ethanol, and extracting at 80 deg.C under reflux for 3 times (45 min each time); mixing the extractive solutions.

(2) Concentrating the extractive solution until no alcohol smell exists, adding 200ml water for dissolving, adding into 300g polyamide column, and eluting with 2000ml distilled water;

(3) Collecting water eluent, concentrating the eluent into thick paste with the density of 1.10, adding 200ml of absolute ethanol, and heating to dissolve the thick paste; filtering while hot, removing insoluble substances, cooling the filtrate, and crystallizing to obtain light yellow powder;

(4) Adding 80ml anhydrous ethanol into pale yellow powder, heating to dissolve, filtering while hot, discarding insoluble substances, cooling the filtrate, and recrystallizing to obtain colorless needle crystal white azalea 4.5g with purity of 98%.

Claims

1. A method for extracting and separating white rhododendron from rhododendron septemlobum leaves comprises the following steps:

(1) Adding the rhododendron flofolium powder into petroleum ether for refluxing; air drying the residue, adding into anhydrous ethanol, reflux extracting for 3 times, and mixing extractive solutions; in the petroleum ether reflux, the ratio of the longshu rhododendron leaf powder to the petroleum ether is 0.1-0.3 g/ml, the reflux temperature is 65-90 ℃, and the reflux time is 1-2h; reflux-extracting the residue in ethanol at 70-80 ℃ for 40-45min each time, wherein the feed liquid ratio of the residue to the ethanol is 0.05-0.2g/ml;

(2) Concentrating the extractive solution until no alcohol smell exists, adding water for dissolving, adding into polyamide column, and eluting with distilled water;

(3) Collecting water eluent, concentrating the water eluent into thick paste with the density of 1.05 to 1.15, adding absolute ethyl alcohol, and heating to dissolve the thick paste; filtering while hot, removing insoluble substances, cooling the filtrate, and crystallizing to obtain light yellow powder;

2. The method of claim 1, wherein the extraction and isolation of rhododendron white from a leaf of Rhododendron moulmainense comprises: in the step (2), the dosage of the polyamide is 0.25 to 1 time of the mass of the rhododendron flosum leaves; the water consumption for elution is 5 to 15 times of the mass of the polyamide.