Preparation of liensinine, isoliensinine and methylliensinine extracted from lotus seed

A kind of technology of lysinine and isiensinine, applied in directions such as organic chemistry, can solve problems such as difficulty in large-scale production, tailing, and difficulty in forming crystallization, and achieves a separation environment that is relaxed, peak-type resolution, and no loss of samples. Effect

Inactive Publication Date: 2005-02-23
ZHEJIANG UNIV
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  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the chemical properties of these three phenolic alkaloids are unstable, easily oxidized, and difficult to form crystals
Therefore, when using traditional separation techniques such as thin-layer chromatography, column chromatography, and high-performance liquid chromatography, tailing, pollution, and loss often occur due to the adsorption of solid carriers, and it is difficult to obtain relatively high-purity compound monomers.
[0003] Chinese patent CN1117735C discloses a method for extracting and purifying isoliensinine and liensinine from lotus seeds. This method is to salt the total alkaloids of lotus seeds and crystallize them step by step. The operation steps are cumbersome and difficult to produce on a large scale.

Method used

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  • Preparation of liensinine, isoliensinine and methylliensinine extracted from lotus seed
  • Preparation of liensinine, isoliensinine and methylliensinine extracted from lotus seed
  • Preparation of liensinine, isoliensinine and methylliensinine extracted from lotus seed

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] 1. Soak 12kg of dried lotus seed heart powder with 10L of 95% ethanol at room temperature for 48 hours, suction and filter out the solvent, add 10L of 95% ethanol to the filter residue, repeat the above operation three times, combine the extracts and reduce them with a rotary evaporator. Concentrate under pressure to form an extract, and the concentration temperature is 40°C. The obtained extract was dissolved with 4L of 1.5% hydrochloric acid, filtered with suction, and the pH of the filtrate was adjusted to 8.5 with 10% ammonia water, and a pale yellow precipitate was precipitated. Collect the precipitated pale yellow precipitate to obtain 85g crude lotus seed alkaloid. HPLC analysis (such as figure 1 , among the figure 1 is liensinine, 2 is isoliensinine, and 3 is methyl-liensinine) shows that the contents of three main components are respectively 15.4%, 15.9%, 47.6%.

[0020] 2. Separating lotus seed alkaloid extract with countercurrent chromatography. Use petrol...

Embodiment 2

[0043] The preparation method of the crude alkaloid of lotus seed is the same as in Example 1, and the extract of lotus seed alkaloid is separated by countercurrent chromatography. Prepare a two-phase solvent with ethyl acetate, carbon tetrachloride, methanol and water in a volume ratio of 1:6:4:1, and separate the upper and lower phases by standing in a liquid separation container. Dissolve 5850 mg of crude alkaloids of lotus root in 15 ml of the upper phase and 15 ml of the lower phase to form a sample solution. The internal diameter of the countercurrent chromatographic column is 4mm, and the column volume is 1600ml. The above phase is used as the stationary phase, and the lower phase is the mobile phase. After the separation column of the countercurrent chromatograph is filled with the stationary phase, the sample solution is injected into the sampling loop of the countercurrent chromatograph, and the countercurrent chromatograph is turned on at a speed of 450 rpm. The fl...

Embodiment 3

[0045]The preparation method of the crude alkaloid of lotus seed is the same as in Example 1, and the extract of lotus seed alkaloid is separated by countercurrent chromatography. Prepare a two-phase solvent with diethyl ether, ethyl acetate, carbon tetrachloride, methanol and water in a volume ratio of 1:1:7.5:5:1, and separate the upper and lower phases by standing in a liquid separation container. Dissolve 150 mg of the crude alkaloid of lotus root in 1.5 ml of the upper phase and 1.5 ml of the lower phase to form a sample solution. The internal diameter of the countercurrent chromatographic column is 2mm, and the column volume is 380ml. The above phase is used as the stationary phase, and the lower phase is the mobile phase. After the separation column of the countercurrent chromatograph is filled with the stationary phase, the sample solution is injected into the sampling loop of the countercurrent chromatograph, and the countercurrent chromatograph is turned on at a spee...

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Abstract

A process for preparing liensinine, iso liensinine and methyl liensinine from the core of lotus seed by counterflow chromatography method features that its separating solvent is the mixture of two or more in n-alkanes, halohydrocarbon, emtrol, lipone, fatty ester, ether and water.

Description

technical field [0001] The invention relates to a method for separating and preparing high-purity monomer liensinine, isoliensinine and methyl-liensinine from lotus seeds by using chromatography. Background technique [0002] Liensinine, isoliensinine, and methyl-liensinine are the main alkaloids of lotus root. Lianzixin is the germ of the seeds of Nymphaeaceae, which is one of the important traditional Chinese medicines in my country. It has the functions of clearing heart-fire, lowering blood pressure, and strengthening the heart. A large number of studies have shown that the active ingredients of lotus seed heart are these three alkaloids. Due to the outstanding efficacy of these three alkaloids in cardiovascular and cerebrovascular and other aspects, the separation and preparation of high-purity compound monomers has become an important content of research. However, the chemical properties of these three phenolic alkaloids are unstable, easy to oxidize, and difficult t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D217/20
Inventor 潘远江吴世华
Owner ZHEJIANG UNIV
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