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Preparation method of 5-hydroxytryptamine derivatives from safflower seed meal by high-speed countercurrent chromatography

A technology of high-speed countercurrent chromatography and safflower seed meal is applied in the field of separation of natural medicines and achieves the effects of good repeatability, simple process and convenient operation.

Active Publication Date: 2016-03-30
CHINA ACAD OF SCI NORTHWEST HIGHLAND BIOLOGY INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The industrial production of 5-hydroxytryptamine derivatives separated from safflower by high-speed countercurrent chromatography has not yet been reported in domestic and foreign literature and patents

Method used

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  • Preparation method of 5-hydroxytryptamine derivatives from safflower seed meal by high-speed countercurrent chromatography
  • Preparation method of 5-hydroxytryptamine derivatives from safflower seed meal by high-speed countercurrent chromatography
  • Preparation method of 5-hydroxytryptamine derivatives from safflower seed meal by high-speed countercurrent chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] 1. Preparation of Crude Extract of 5-Hydroxytryptamine Derivatives

[0034] Take 300g of safflower seed meal and reflux extraction with absolute ethanol (liquid-to-material ratio: 15:1) for 1h, extract 3 times to combine the extract, evaporate to dryness with a rotary evaporator, dissolve in 500ml of 80% methanol, extract with an equal volume of n-hexane, and take the methanol phase Evaporate to dryness, dissolve in 300ml of ethyl acetate, then extract with an equal volume of water, and take the ethyl acetate phase and evaporate to dryness for later use.

[0035] 2. Preparation of 5-hydroxytryptamine derivatives by high-speed countercurrent separation

[0036] Prepare a two-phase solvent system of chloroform-methanol-0.1mol / L HCL water (1:1:1, v / v) in a separatory funnel, shake well and let stand overnight. The lower phase was the stationary phase, and the upper phase was the mobile phase, which were ultrasonically degassed for 30 min before use. Take 100 mg of the sa...

Embodiment 2

[0043] 1. Preparation of Crude Extract of 5-Hydroxytryptamine Derivatives

[0044] The preparation of the crude extract of 5-hydroxytryptamine derivatives is the same as in Example 1.

[0045] 2. Preparation of 5-hydroxytryptamine derivatives by high-speed countercurrent separation

[0046] Prepare a chloroform-methanol-0.1mol / L HCL water (3.5:4:4.5, v / v) two-phase solvent system in a separatory funnel, shake it well and let it stand overnight. The lower phase was the stationary phase, and the upper phase was the mobile phase, which were ultrasonically degassed for 30 min before use. Take 120mg of the sample powder to be separated, shake it and dissolve it completely in 10mL of the lower phase solution, and set it aside.

[0047] The lower phase of the solvent system was pumped into the main unit with a flow rate of 15 mL / min to fill the separation solenoid, and the circulating water bath was turned on and the temperature was set to 25 °C. Turn on the power of the main engi...

Embodiment 3

[0049] 1. Preparation of Crude Extract of 5-Hydroxytryptamine Derivatives

[0050] The preparation of the crude extract of 5-hydroxytryptamine derivatives is the same as in Example 1.

[0051] 2. Preparation of 5-hydroxytryptamine derivatives by high-speed countercurrent separation

[0052] Prepare a two-phase solvent system of chloroform-methanol-0.1mol / L HCL water (1:1:1, v / v) in a separatory funnel, shake well and let stand overnight. The lower phase was the stationary phase, and the upper phase was the mobile phase, which were ultrasonically degassed for 30 min before use. Take 100 mg of the sample powder to be separated, shake it and dissolve it completely in 10 mL of the lower phase solution, and set it aside.

[0053] The lower phase of the solvent system was pumped into the main unit with a flow rate of 15 mL / min to fill the separation solenoid, and the circulating water bath was turned on and the temperature was set to 25 °C. Turn on the power of the main engine an...

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Abstract

The invention relates to a separation and preparation method of a natural medicine, and particularly relates to a method for separating and preparing two 5-hydroxytryptamine derivatives from safflower seed meal by high-speed countercurrent chromatography. The solid phase and mobile phase of high-speed countercurrent chromatography are mixed by chloroform, methanol and 0.1mol / L HCL water before layering, wherein the lower phase is used as a solid phase, and the upper phase is used as a mobile phase. In the method provided by the invention, without necessity of using a solid-phase carrier and without irreversible adsorption, the method is convenient to operate, the conditions are fixed, the repetition is easy, sample loss and pollution are avoided, the 5-hydroxytryptamine derivatives are efficiently and quickly prepared at a low cost, the purity of the obtained N-(p-coumaroyl) 5-hydroxytryptamine and feruloyl 5-hydroxytryptamine monomers can exceed 95%, and industrial production can be performed.

Description

technical field [0001] The invention relates to a method for separating natural medicines, in particular to a method for separating and preparing two serotonin derivatives from safflower seed dregs by high-speed countercurrent chromatography. Background technique [0002] Safflower (Carthamustinctorius L.) is a plant of the Compositae family, which is an economic crop with both medicine, oil, dye and feed. Safflower seeds, commonly known as "Baipingzi" in traditional Chinese medicine, are the seeds of safflower. Safflower seed meal is the waste left after the oil is extracted from safflower seeds. It is mostly used as fertilizer and feed, and there are few studies on its chemical components. In recent years, some trace components in safflower seed meal have been studied abroad, and it is found that 5-hydroxytryptamine derivatives in safflower seed meal have strong free radical scavenging and active antioxidant properties, and can regulate the immune response in the human bo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D209/16
CPCC07D209/16
Inventor 丁晨旭李文聪王小艳张秋龙王洪伦索有瑞
Owner CHINA ACAD OF SCI NORTHWEST HIGHLAND BIOLOGY INST