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Method for abstracting and separating iridoid compound monomer from oldenlandia diffusa

A technology of Hedyotis diffusa and iridoids is applied in the field of phytochemistry, can solve the problems of high cost, low product yield, complicated methods and the like, and achieves low cost, high yield, easy control and operation. Effect

Active Publication Date: 2008-01-02
SHANGPHARMA INNOVATION JIANGXI CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The above separation methods all use more than three steps of column chromatography, and use a large amount of organic solvents that are not easy to recycle. The method is complicated, the cost is high, and the product yield is low.

Method used

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  • Method for abstracting and separating iridoid compound monomer from oldenlandia diffusa
  • Method for abstracting and separating iridoid compound monomer from oldenlandia diffusa

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 1Kg of pulverized Hedyotis diffusa is heated and refluxed with ethanol aqueous solution of 95% ethanol to extract twice, each time for 2 hours, the weight ratio of said Hedyotis diffusa to ethanol aqueous solution is 1: 1.5, filter and concentrated to obtain extract (I) (relative density 1.197, 60°C), dissolved in water, filtered, and the filtrate was concentrated under reduced pressure to obtain extract (II) (relative density 1.156, 60°C). The extract (II) is dissolved in an aqueous ethanol solution with a volume concentration of ethanol of 20%, and the weight ratio of the extract (II) to the aqueous ethanol solution is 1:5; on MCI gel CHP 20P (styrene) macroporous resin column chromatography, The weight ratio of extract (II) and macroporous resin MCI gel CHP 20P is 1: 1; With 20%, 30%, 40%, 50%, 60% ethanol gradient elution, thin-layer chromatography tracking detection, at 50 There is a large spot in the eluting part of % ethanol, after collecting the spot and concent...

Embodiment 2-6

[0035] Embodiment 2-6 Extraction, separation steps are referring to embodiment 1, what adopted in the embodiment is pulverized Hedyotis diffusa 1kg, the extraction of each example, separation conditions see table 1 below

[0036] Table 1

[0037] Example

[0038] 4

[0039] 6

Embodiment 7

[0040] Example 7 Inhibitory Action Test on Cancer Cell Lines

[0041] Test substance: E-6-O-coumaroyl gallinosin methyl ester

[0042] Positive control: 5-fluorouracil (5-FU)

[0043] Cell lines: lung cancer A549 and liver cancer SMMC-7721 (purchased from Shanghai Institutes for Biological Sciences, Chinese Academy of Sciences)

[0044] experimental method:

[0045] E-6-O-coumaroyl gallinacein methyl ester is made into mother liquor with culture medium (10 -4 mol / L), and then diluted with culture medium to different concentrations before use.

[0046] 8 MTT (thiazole blue) test:

[0047] A549 and SMMC-7721 cells were inoculated into 96-well cell culture plates at 3,000 and 5,000 cells per well, respectively. After 24 hours of culture, the supernatant was discarded, and 100 μL of culture solution containing different concentrations of drugs was added to each well, with concentrations of 10 -4 , 10 -5 , 10 -6 , 10 -7 , 10 -8 mol / L, the same concentration of 5-fluorourac...

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PUM

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Abstract

The invention relates to a method for extracting and separating more than 90% iridoid glycoside compound monomer from efflorescence snake tongue grass, wherein the iridoid glycoside compound monomer of efflorescence snake tongue grass is E-6-0-coumaricacetate paederoside methyl ester. The method comprises the following steps: (1)putting the disintegrated efflorescence snake tongue grass in the primary alcohol aqueous solution in order to heat, reflux and extract; filtering; getting the concrete (I)by concentrating; adding the water in order to dissolve; filtering; getting the concrete (II)by concentrating; (2)dissolving the concrete (II)with the secondary alcohol aqueous solution; separating with macroreticular resin column; eluting with the tertiary alcohol aqueous solution; concentrating the eluent; getting the primary product; (3)proceeding with chromatography with Sephadex LH-20 column after dissolving the primary product with the fourth alcohol aqueous solution; proceeding with gradient elution with the fifth alcohol solution; concentrating; crystallizing; getting the product E-6-0-coumaricacetate paederoside methyl ester. The method can recycle the column material and solvent, which doesn't pollute the environment, has the low cost, the high product efficient and the easy operation, and is fit for the small-scale extraction separation of the laboratory and the industry extraction separation.

Description

technical field [0001] The present invention relates to the field of phytochemistry, in particular to E-6-O-coumaroyl gallinacein, an iridoid compound monomer extracted from Hedyotis diffusa with an isolation purity of more than 90%. Methyl ester method. Background technique [0002] Hedyotis diffusa Willd. (Hedyotis diffusa Willd.) is the whole herb of Hedyotis diffusa Willd., a plant of Rubiaceae Auricularia. The main production is distributed in Guangdong, Guangxi, Fujian and other places. Its chemical composition is mainly E-6-O-coumar Iridoids such as acyl stilidin methyl ester, triterpenoids such as oleanolic acid, and flavonoids such as rutin. Hedyotis diffusa uses the whole plant as medicine, which has the functions of clearing away heat and detoxifying, diuresis, reducing swelling, promoting blood circulation and relieving pain. tumor. However, there are few studies on the quality control of Hedyotis diffusa and various medicines made from it; quantitative oleano...

Claims

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Application Information

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IPC IPC(8): C07H17/04C07H1/08
Inventor 孙全忠孙斌陈伟
Owner SHANGPHARMA INNOVATION JIANGXI CO LTD
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