Method of obtaining and separating rosmarinic acid, apigenin and luteolin from elsholtzia haichowensis

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

Inactive Publication Date: 2013-06-05
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 of obtaining and separating rosmarinic acid, apigenin and luteolin from elsholtzia haichowensis
  • Method of obtaining and separating rosmarinic acid, apigenin and luteolin from elsholtzia haichowensis
  • Method of obtaining and separating rosmarinic acid, apigenin and luteolin from elsholtzia haichowensis

Examples

Experimental program
Comparison scheme
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 flowering branches and leaves of Rhizoma haizhou harvested at the full bloom stage and grind them into dry powder (moisture content is less than 0.5%, weight ratio), and pass through a 100-mesh sieve. Take the above 500g dry powder, put it into a 10L plastic bucket, add 5L of 95% (V / V) ethanol, stir evenly and soak for 3 days until the material is completely absorbed, treat with 40KHz ultrasonic frequency for 1 hour, and filter with suction 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 from the three extractions were combined; then concentrated in vacuo at 45°C to obtain 126.1 g of extract ① (ie, cru...

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 and refining 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 development system to carry out pressurized column elution, a total of 400ml eluent is required, collect the effluent from each tube (collect 1 tube per 10ml), and keep Carry out TLC spot 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 indica...

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 20ml 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 characteristic peaks of apigenin (purity 100%) are 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 (125 MHz, DMSO-d 6 ) δ(ppm): 182.208, 164.562, 164.179, 161.914, 161.547, 157.773, 128.927, 121.653, 116.369, 116.369, 104.126, 103.37, 99.26, 194.434 The main characteristic pea...

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Abstract

The invention discloses a method of obtaining and separating rosmarinic acid, apigenin and luteolin from elsholtzia haichowensis. The method of obtaining and separating the rosmarinic acid, the apigenin and the luteolin from the elsholtzia haichowensis includes the following steps: (1) ethanol digestion: drying and grinding the obtained flowering branches and leaves of the elsholtzia haichowensis in the blooming period, and obtaining brownish black extractum through digestion and extraction; (2) conducting coarse separation of macroporous resin of brownish black extractum and obtaining yellowish-brown extractum through concentration; (3) conducting separation of polyamide columns of the brownish black extractum, and respectively obtaining extractum A, extractum B and extractum C; (4) respectively conducting chromatographic purification refining of the extractum A, the extractum B and the extractum C, and obtaining the the rosmarinic acid, the apigenin and the luteolin correspondingly. The method of obtaining and separating the rosmarinic acid, the apigenin and the luteolin from the elsholtzia haichowensis can obtain highly purified rosmarinic acid, apigenin and luteolin.

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): C07C69/732C07C67/48C07C67/56C07D311/30C07D311/40
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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