A kind of lignans from tianmuqionghua branches and leaves, its extraction method and application

A technology of agarwood lignans and extraction methods, which is applied in the field of natural products, can solve the problem of not being able to obtain high-purity agarwood branches and leaves lignans compound monomers with anti-atherosclerotic activity, and achieve less pollution discharge and structural clear effect

Active Publication Date: 2019-01-25
TAISHAN MEDICAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to provide a method for extracting the lignan components from the branches and leaves of Qionghua Tianmu, aiming at solving the problem that the current extraction method cannot obtain high-purity monomers of lignans from the branches and leaves of Qionghua Tianmu and the activity of anti-atherosclerosis

Method used

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  • A kind of lignans from tianmuqionghua branches and leaves, its extraction method and application
  • A kind of lignans from tianmuqionghua branches and leaves, its extraction method and application
  • A kind of lignans from tianmuqionghua branches and leaves, its extraction method and application

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Experimental program
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Effect test

Embodiment 1

[0046] After crushing 20Kg of dried branches and leaves of Qionghua Tianmu, cold-soak in 50L of 95% ethanol at room temperature for 48-72 hours for percolation extraction. The ethanol extract is concentrated under reduced pressure with a 30L large-scale rotary evaporator, and the evaporated ethanol is poured back into the percolation jar for cold soaking 24 to 48 hours; carry out second percolation extraction on the medicinal powder, second concentration, pour the evaporated ethanol back into the percolation tank for cold soaking for 24 to 48 hours; perform third percolation extraction on the medicinal powder, three times of concentration, and recover ethanol , until the concentrated solution has no alcohol smell, 2000g of total extract is obtained, and ethanol is recovered. Suspend the extract in warm water with a constant temperature ultrasonic instrument, sequentially extract with 1 to 1.5 times of petroleum ether, chloroform, ethyl acetate and n-butanol, and concentrate und...

Embodiment 3

[0050] The structure determination of embodiment 3 monomer magnolanin (compound 1)

[0051] White powder (chloroform). ESI-MS m / z: 417[M+H]+, the molecular formula is C 23 h 28 o 7 . 1H-NMR (400MHz, CDCl 3 )δ: 3.10(2H,m,H-1,5),3.82,3.86,3.88(each,3H,s,OMe),3.86(6H,s,OMe),3.92,4.27(each 2H,m,H -4,8); 4.74(2H,m,H-2,6),6.81-6.90(5H,m,Ar-H).13C-NMR(100MHz,CDCl3)δ:54.3(C-1),54.6 (C-5), 56.1(OMe), 56.4(OMe), 61.2(OMe), 72.0(C-4), 72.2(C-8), 85.9(C-2), 86.3(C-6), 103.0 (C-2″,6″),109.4(C-2′),111.2(C-5′),118.5(C-6′),133.6(C-1′),137.0(C-1″), 137.7 (C-4″), 148.9 (C-3′), 149.4 (C-4′), 153.7 (C-3″, 5″). For the hydrogen spectrum and carbon spectrum, please refer to the appendix of the manual figure 2 and image 3

Embodiment 4

[0052] The structure determination of embodiment 4 monomer (+)-cineole (compound 2)

[0053] White powder (chloroform). ESI-MS m / z:387[M+H]+, molecular formula is C 22 h 26 o 6 . 1H-NMR (400MHz, CDCl 3 )δ:6.90-6.80(6H,m,Ar-H),3.10(2H,m,H-1,5),4.74(2H,d,J=4.1Hz,H-2,6),4.25(2H ,dd,J=8.9,6.9Hz,H-4α,8α),3.95(2H,dd,J=8.9,6.9Hz H-4β,8β),3.88(6H,s,OCH3×2),3.86(6H ,s,OCH3×2),; 13C-NMR(CDCl3,100MHz)δ:54.4(C-1,5),86.0(C-2,6),71.9(C-4,8),134.6(C- 1′,1″),110.9(C-2′,2″),149.5(C-3′,3″),149.7(C-4′,4″),112.3(C-5′,5″) , 119.3 (C-6′,6″), 56.1 (OCH3×2), 56.2 (OCH3×2). For the hydrogen spectrum and carbon spectrum, please refer to the appendix of the manual Figure 4 and Figure 5 .

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Abstract

The invention discloses a viburnum sargentii branch and leaf lignan, an extraction method and application. The extraction method comprises the steps of smashing dried viburnum sargentii branches and leaves, and the like; using a constant-temperature ultrasonic instrument for suspending an extract with warm water, extracting, and decompress concentrating to obtain an extract; dissolving the extract at a cholorform part in methanol, eluting to remove chlorophyll, carrying out chromatography and purification to obtain 5 different compounds. A monomer lignan obtained through the invention has the purity achieving 96 percent to 99 percent, can be subjected to goal-oriented structural modification, and is applied in pharmaceutical synthesis so as to obtain pharmaceutical molecules with better activity; 5 lignans are firstly extracted from viburnum sargentii , so that an approach for obtaining such natural active ingredients is wider. The extraction method provided by the invention is simple and convenient, easy to separate and recover an organic solvent mixture, less in emission, and suitable for modern fine industrial production. The invention adopts a latest SBC MCI GEL reversion phase chromatography filler, so that the removal rate of chlorophyll is improved from 60 percent to 70 percent to 97 percent to 100 percent. The invention discloses anti-atherosclerosis application of the lignan monomer.

Description

technical field [0001] The invention belongs to the technical field of natural products, and in particular relates to a method and application of extracting lignan components from branches and leaves of Qionghua tianmu. Background technique [0002] Viburnum sargentii is a plant of the genus Viburnum in the family Caprifoliaceae. my country's Heilongjiang, Jilin, Liaoning, northern Hebei, Shanxi, southern Shaanxi, southern Gansu, western Henan, Shandong, southern and western Anhui, northwestern Zhejiang, Jiangxi (Huanglong Mountain), Hubei and Sichuan are all distributed. It tastes sweet, bitter, and flat in nature. It enters the lung, liver, spleen, and kidney meridians. Modern pharmacological studies have shown that the fruit of Qionghua Tianmu can treat chronic bronchitis, cough, phlegm and asthma, and anti-tumor, but there is no report on the extraction method of lignans from Qionghua Tianmu. The present invention is the first to systematically study the chemical compo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D493/04C07D209/12A61K31/343A61K31/34A61P9/10A61K49/00
CPCA61K49/0008C07D209/12C07D493/04
Inventor 朱焰庞现红姚广民
Owner TAISHAN MEDICAL UNIV
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