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Preparation method of highly-pure sesamin monomer and highly-pure sesamolin monomer

A technology of sesamolin and sesamin, which is applied in the field of separation and purification of plant active ingredients, can solve the problems of large separation technology, low preparation efficiency, and difficult preparation volume, and achieve good separation effect, low preparation cost and good reproducibility Effect

Active Publication Date: 2016-10-05
SHANDONG ANALYSIS & TEST CENT +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, there is no patent for the separation of sesamin and sesamolin monomers in China. The existing literature methods for the separation and preparation of high-purity sesamin and sesamolin monomers mainly use repeated silica gel column chromatography, Sephadex LH The limitations of methods such as -20 column chromatography are time-consuming and laborious, polluting the environment, low sample purity, and repeated column chromatography has irreversible adsorption to the sample, and the isolation of high-purity sesamin and sesamin monomers has low preparation efficiency, The cost is high, and it is difficult to develop into a separation technology with a large amount of preparation

Method used

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  • Preparation method of highly-pure sesamin monomer and highly-pure sesamolin monomer
  • Preparation method of highly-pure sesamin monomer and highly-pure sesamolin monomer
  • Preparation method of highly-pure sesamin monomer and highly-pure sesamolin monomer

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Embodiment 1

[0035] Such as figure 1 Shown, the preparation method of high-purity sesamin monomer and sesamin monomer in the present embodiment comprises the following steps:

[0036] (1) Take 1.1 kg of sesame seeds and pulverize them and extract them with 10 L of n-hexane reflux for 3 times, each time for 2 hours, filter with suction, and the filtrate is vacuum rotary evaporated into an oily state to obtain 489.5 g of total extracts;

[0037] (2) Add 500mL of ethanol to the above-mentioned total extract and ultrasonically extract 3 times, each time for 2h, take the supernatant and vacuum rotary evaporation to obtain 10.3g of sesame crude extract (such as Figure 4 shown);

[0038] (3) According to the volume ratio, make petroleum ether: ethyl acetate: methanol: water = 1:0.4:1:0.5 into a refined solvent system, put it in a separatory funnel, shake it up, let it stand for stratification, and wait for a period of equilibrium After a period of time, the upper and lower phases are separated...

Embodiment 2

[0045] The preparation flow chart of sesamin monomer and sesamin monomer is as figure 1 shown.

[0046] 1. Take 1.0kg of sesame seeds, pulverize them and extract them with petroleum ether reflux for 3 times, each time for 2 hours, filter, and concentrate the filtrate under reduced pressure to obtain an extract to obtain a total extract of 460.8g.

[0047] 2. Add 500 mL of methanol to the above total extract and ultrasonically extract 3 times, each time for 2 hours, take the supernatant and vacuum rotary evaporation to obtain 9.5 g of crude sesame extract.

[0048] 3. The selected solvent system for separation is n-hexane: ethyl acetate: methanol: water = 1:0.5:1:0.5, and the rest of the steps are the same as in Example 1. The obtained purity is 99.6% and 98.3% of sesamin and sesamolin monomer 70mg and 6.2mg, and the high-speed countercurrent chromatographic separation ultraviolet spectrogram is shown in image 3 .

Embodiment 3

[0050] The solvent system selected for separation is petroleum ether: propyl acetate: ethanol: water = 1:0.5:1:0.6, and the rest of the steps are the same as in Example 1. 71 mg and 6.4 mg of sesamin and sesamolin monomer with a purity of 99.5% and 98.2% were obtained.

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Abstract

The invention relates to a separation and purification method of plant effective components, and especially relates to a preparation method of a highly-pure sesamin monomer and a highly-pure sesamolin monomer. The preparation method comprises the following steps: 1, carrying out refluxing extraction on sesame; 2, carrying out secondary extraction with a solvent; 3, preparing a purified solvent system by using a component A, a component B, a component C and a component D according to a volume ratio of 1:0.2-1:0.5-3:0.2-1 in order to obtain a stationary phase and a mobile phase; and 4, separating a sample by using a high speed countercurrent chromatograph, the stationary phase and the mobile phase, and collecting target components according to obtained chromatogram in order to respectively obtain the highly-pure sesamin monomer and the highly-pure sesamolin monomer. The preparation method has the advantages of good reappearance, good separation effect, high efficiency, and high purity of sesamin and sesamolin monomer products reaching 98% or above.

Description

technical field [0001] The invention relates to a method for separating and purifying plant effective components, in particular to a method for preparing high-purity sesamin and sesamin monomer. Background technique [0002] Sesamin and sesamolin are a class of lignan compounds present in sesame and are the main active ingredients of sesame. Sesamin C 20 h 18 o 6 , with a melting point of 121-122°C, and its content accounts for about 0.2%-0.5% of sesame. A large number of studies have shown that sesamin can inhibit viruses such as influenza virus, Sendai virus and Mycobacterium tuberculosis, and has the functions of lowering cholesterol, promoting fat oxidation, and inhibiting fat synthesis. , treatment of bronchitis, anti-hypertensive, anti-cancer and other effects. It is used as an additive for pyrethrins in agriculture. Sesamolin is also one of the main lignans in sesame, molecular formula C 20 h 18 o 7 , melting point 93-94 ℃, pharmacological research results sho...

Claims

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Application Information

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IPC IPC(8): C07D493/04
Inventor 王岱杰周晓晶王尉王晓耿岩玲段文娟林楠
Owner SHANDONG ANALYSIS & TEST CENT
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