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Method for extracting bibenzyl compounds from dendrobium officinale and application thereof

A technology of dendrobium candidum and compounds, applied in the direction of active ingredients of heterocyclic compounds, food ingredients containing natural extracts, applications, etc., can solve the problems of incomplete and in-depth chemical components and pharmacological effects, and achieve easy large-scale production and application, liver cancer Cytostatic activity Safe, non-toxic, strong activity effect

Active Publication Date: 2020-05-01
ZHEJIANG UNIV +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] At present, the research on the chemical constituents and pharmacological effects of Dendrobium candidum is not comprehensive and in-depth. The types of compounds extracted from Dendrobium candidum disclosed in the existing literature are few. In order to solve the above problems, it is urgent to find a new extraction method. Extract more active compounds that are beneficial to the human body

Method used

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  • Method for extracting bibenzyl compounds from dendrobium officinale and application thereof
  • Method for extracting bibenzyl compounds from dendrobium officinale and application thereof
  • Method for extracting bibenzyl compounds from dendrobium officinale and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] Embodiment 1: the preparation of compound (1)

[0060] (1) Take 11 kg of dried Dendrobium candidum, soak and extract 2 times with 27L 95% ethanol, filter the leachate, combine the obtained filtrate, concentrate to 1.25L with a rotary evaporator after high-speed centrifugation, and continue to recover the concentrated liquid under reduced pressure to obtain 485.6g leachate paste;

[0061] (2) Load the extract by dry method, pass through HP-20 macroporous resin column chromatography (40cm×15cm), the eluent is ethanol and water with a volume ratio of 0:100~95:5, and each part is eluted 5 column volumes, respectively get water parts, ethanol with a volume ratio of 10:90, 20:80, 30:70, 40:60, 50:50, 60:40, 70:30, 80:20, 95:5 and water part; ethanol and water with a volume ratio of 50:50; ethanol and water with a volume ratio of 60:40; ethanol and water parts with a volume ratio of 70:30;

[0062] (3) Collect the sample after concentration and drying of the ethanol and wate...

Embodiment 2

[0067] Embodiment 2: the preparation of compound (2)

[0068] The extraction, concentration, macroporous resin enrichment, reversed-phase resin column chromatography, silica gel column chromatography, and separation process of gel column chromatography of Dendrobium officinale are the same as in Example 1. The difference is that after Sephadex LH-20 gel column chromatography (methanol) elution, the second chromatographic peak part is collected, concentrated under reduced pressure and separated by preparative liquid phase (C18, 250mm×10mm, 5 μm) to obtain (2) compound ( 50% acetonitrile, t R 57min).

[0069] Compound (2) is a colorless jelly, soluble in methanol and chloroform. After the sample TLC is developed, the color of 5% ferric chloride ethanol solution is gray, and the color of 10% sulfuric acid ethanol solution is black.

[0070] 1 H NMR (600MHz, CD 3 OD)δ H 6.71(1H,d,J=8.0Hz,H-5′),6.66(1H,d,J=1.8Hz,H-2′),6.60(1H,dd,J=8.0,1.8Hz,H-6 '), 6.39 (2H, s, H-2, 6), 3....

Embodiment 3

[0072] Embodiment 3: the preparation of compound (3)

[0073] Step (1), (2) are with embodiment 1;

[0074] (3) Collect the concentrated and dried samples of ethanol and water eluent with a volume ratio of 50:50, use MCI CHP-20P reverse phase resin column (20cm×3cm) chromatography, and use ethanol-water solvent system (30:70, 40:60, 50:50, 60:40, 70:30, 80:20, 90:10, 95:5) were eluted in sections, and the ethanol and water eluted fractions with a volume ratio of 40:60 were collected and concentrated to dryness Afterwards, it was eluted by Sephadex LH-20 gel column (220cm×2cm) chromatography (methanol), and 4 fractions were obtained. The third fraction was collected, concentrated under reduced pressure and separated by preparative liquid phase (C18, 250mm×10mm, 5 μm). Using methanol and water with a volume ratio of 59:41 as the mobile phase and a flow rate of 3ml / min, the chromatographic peaks with a retention time of 30min were collected, and the solvent was recovered under r...

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Abstract

The invention discloses a method for extracting bibenzyl compounds from dendrobium officinale, which comprises the following steps: carrying out alcohol extraction and concentration on dendrobium officinale to obtain an extract, eluting with an ethanol solution through macroporous resin, respectively collecting the eluates, and performing separation and purification continuously to obtain the bibenzyl compounds. The invention also discloses an application of the bibenzyl compound extracted from dendrobium officinale for the first time in preparation of a medicine for preventing or / and treatingcervical cancer or liver cancer and an application in preparation of a health care product for immunoregulation and / or improvement of microcirculation and / or improvement of life quality. The bibenzylcompounds are extracted from dendrobium officinale for the first time and have good HeLa and HepG2 inhibitory activity. The extraction method is simple to operate, good in separation effect and easyfor large-scale production and application.

Description

technical field [0001] The invention belongs to the field of traditional Chinese medicine health food, and in particular relates to a method for extracting bibenzyl compounds from dendrobium officinale and an application thereof. Background technique [0002] Dendrobium officinale has a long history of application in China and Southeast Asia as a health food and nutritional product. "Chinese Pharmacopoeia" records that Dendrobium candidum has the effect of "benefiting the stomach and promoting body fluid, nourishing yin and clearing away heat", and is often used for "fever disease, fluid injury, dry mouth, polydipsia, insufficient stomach yin, and retching due to lack of food." [0003] The chemical components of Dendrobium officinale include polysaccharides, bibenzyls, alkaloids, phenanthrenes, flavonoids, terpenoids, phenolic acids and other components. A large number of extraction methods have been recorded in the existing literature. For example, the Chinese invention pa...

Claims

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Application Information

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IPC IPC(8): C07C41/34C07C43/23C07D319/20C07D317/54A61K31/36A61K31/357A61K31/09A61P35/00A23L33/105
CPCA23V2002/00A61K31/09A61K31/357A61K31/36A23L33/105A61P35/00C07C41/34C07D317/54C07D319/20C07C43/23A23V2200/30A23V2200/324A23V2250/21
Inventor 陈云龙任刚张征肖川云黄彩平徐程蒋欣杭陈汉民黄方亮张麝龙吴运荣
Owner ZHEJIANG UNIV
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