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Method for extraction and separation of rosmarinic acid, apigenin and luteolin in elsholtzia splendens

A technology of rosmarinic acid and luteolin, applied in the field of biological resource utilization of natural products

Inactive Publication Date: 2012-09-12
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] So far, there is no domestic report about the method of simultaneously extracting and separating rosmarinic acid, apigenin and luteolin from the environmental specific plant Cyperus haizhou

Method used

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  • Method for extraction and separation of rosmarinic acid, apigenin and luteolin in elsholtzia splendens
  • Method for extraction and separation of rosmarinic acid, apigenin and luteolin in elsholtzia splendens
  • Method for extraction and separation of rosmarinic acid, apigenin and luteolin in elsholtzia splendens

Examples

Experimental program
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Effect test

Embodiment 1

[0040] Embodiment 1, the solvent extraction and the separation of the dry powder of mosaic and leaf in the Rhizoma haizhou of the present invention

[0041] (1), alcohol extraction:

[0042] Air-dry the flower branches and leaves of Cyperus haizhou harvested in the full bloom stage and grind them into dry powder (moisture content is lower than 0.5%, weight ratio), and pass through a 100-mesh sieve. Take the above 500g of dry powder, put it in a 10L plastic bucket, add 5L of 95% (V / V) ethanol, stir evenly and soak for 3 days until the material is completely imbibed, treat with 40KHz ultrasonic frequency for 1 hour, and suction filter to obtain the filtrate. Repeat the above-mentioned process twice for the residue obtained by suction filtration (that is, replace the dry powder with the residue, and repeat the above-mentioned leaching). The filtrates obtained by leaching three times were combined; then concentrated in vacuo at 45° C. to obtain 126.1 g of extract ① (ie, crude ext...

Embodiment 2

[0056] Example 2, thin-layer silica gel purification and refining of apigenin, luteolin and rosmarinic acid in Herba pilosula of the present invention

[0057] (1) Thin-layer silica gel purification of apigenin.

[0058] Dissolve 50 g of 200-mesh silica gel in 250 ml of ethyl acetate, stir to remove air bubbles, and pack the column under pressure.

[0059] 0.782g of extract A obtained in Example 1 was dissolved with 4ml of methanol, and 2g of silica gel was added to mix the sample, spin-dried and then mounted on the top of the column. Use the volume ratio of ethyl acetate: methanol: formic acid = 20:3:1 as the developing system to carry out pressurized column elution, a total of 400ml of eluent is required, collect the effluent from each tube (collect 1 tube per 10ml), and Carry out TLC point plate tracking, blue fluorescence under ultraviolet light, 1% AlCl 3 The solution is bright yellow and the iodine-fumed silica gel plate has no impurities, and the three indicators shal...

Embodiment 3

[0064] Embodiment 3, identification of the chemical structure of apigenin, luteolin, and rosmarinic acid in A. haizhouensis of the present invention

[0065] The light yellow compounds (compounds a, b, c) obtained in Example 2 were dissolved in 20 ml of ultrapure water, frozen at -40°C for 2 hours, and dried in vacuum freezer (-80°C) to obtain the product. They were dissolved in deuterated DMSO, and the H-NMR and C-NMR spectra were measured, and the infrared spectrum was measured by the tablet method, which were used to identify the structure. Data are as follows:

[0066] The proton nuclear magnetic resonance spectrum and carbon spectrum of apigenin (purity 100%) are as figure 2 As shown, the characteristic peaks are assigned as follows: 1 H-NMR (500MHz, DMSO-d 6 )δ(ppm): 12.975(s, 1H), 10.605(s, 1H), 7.936(d, J=8.0Hz, 2H), 6.938(d, J=8.3Hz, 2H), 6.785(s, 1H) , 6.487(s, 1H), 6.199(s, 1H). 13 C-NMR (125MHz, DMSO-d 6 )δ (ppm): 182.208, 164.562, 164.179, 161.914, 161.547...

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Abstract

The invention discloses a method for extraction and separation of rosmarinic acid, apigenin and luteolin in elsholtzia splendens. The method comprises the steps of: (1) ethanol immersion extraction: performing air drying, smash, immersion extraction and extraction on branches and leaves of elsholtzia splendens harvested in the full-bloom stage to obtain a brownish black extractum; (2) performing macroporous resin coarse separation and concentration on the brownish black extractum to obtain a yellowish-brown extractum; (3) performing polyamide column separation on the obtained yellowish-brown extractum to obtain an extractum A, an extractum B and an extractum C; and (4) performing silica-gel column chromatography purification and refinement on the extractum A, the extractum B and the extractum C to obtain the apigenin, the apigenin and the rosmarinic acid correspondingly. Highly purified rosmarinic acid, apigenin and luteolin can be obtained by adopting the method provided in the invention.

Description

technical field [0001] The invention belongs to the field of biological resource utilization of natural products, and relates to a method for extracting and separating rosmarinic acid, apigenin and luteolin in an environment-specific plant A. haizhouensis. Background technique [0002] Extracting anti-tumor active ingredients from plants has always been a hot field in the research of natural product chemistry. The active ingredients of natural anti-tumor drugs are various, mainly alkaloids, traditional Chinese medicine polysaccharides, polyphenols, proteins, quinones, terpenes, etc. Plant polyphenols have been proved to have anti-tumor effects. According to reports, leukemia cells, lung tumor cells and breast cancer cells were selected as research objects, and it was found that even a small amount of polyphenols can inhibit the enzymes in tumor cells, and these enzymes are important for the production of "signal" molecules that trigger tumor cell growth. Essential (German s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/732C07C67/56C07C67/58C07D311/30
Inventor 彭红云邢严张良章国林申有青王会平曾卫卫
Owner ZHEJIANG UNIV
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