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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  • 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-co

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

Examples

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Example Embodiment

[0034] Example 1

[0035] Such as figure 1 As shown, the preparation method of high-purity sesamin monomer and sesalin monomer in this embodiment includes the following steps:

[0036] (1) Take 1.1 kg of sesame seeds, crush them, and extract them with 10L n-hexane refluxing for 3 times, 2h each time, suction filtration, and vacuum rotary evaporation of the filtrate into an oily state to obtain a total extract of 489.5g;

[0037] (2) Add 500 mL of ethanol and ultrasonically extract the above total extract 3 times, 2h each time, take the supernatant and vacuum rotary evaporate to obtain 10.3g crude sesame extract (e.g. Figure 4 Shown);

[0038] (3) According to the volume ratio, mix petroleum ether: ethyl acetate: methanol: water=1:0.4:1:0.5 into a refined solvent system, place it in a separatory funnel, shake well, stand still for layering, wait for a period of equilibrium After time, separate the upper and lower phases, the upper layer is the stationary phase, and the lower layer is ...

Example Embodiment

[0044] Example 2

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

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

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

[0048] 3. The solvent system selected for separation is n-hexane: ethyl acetate: methanol: water=1:0.5:1:0.5, and the remaining steps are the same as in Example 1. 70mg and 6.2mg of sesamin and sesalin monomers with purity of 99.6% and 98.3% were obtained. The UV spectra of high-speed countercurrent chromatography are shown in image 3 .

Example Embodiment

[0049] Example 3

[0050] The solvent system selected for separation is petroleum ether: propyl acetate: ethanol: water=1:0.5:1:0.6, and the remaining steps are the same as in Example 1. 71 mg and 6.4 mg of sesamin and sesalin monomer with 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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