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Method for separation and preparation of spermidines from safflower by employing high-speed counter-current chromatography

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

Inactive Publication Date: 2014-01-15
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 spermidine compounds 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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  • Method for separation and preparation of spermidines from safflower by employing high-speed counter-current chromatography
  • Method for separation and preparation of spermidines from safflower by employing high-speed counter-current chromatography
  • Method for separation and preparation of spermidines from safflower by employing high-speed counter-current chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] 1. Preparation of safflower spermidine crude extract

[0040] Take 500 g of safflower, add 70% alcohol according to the liquid-to-material ratio of 15:1, and extract under reflux at 60 °C for 3 times, each time for 2 h, combine the extracts and concentrate to dryness under reduced pressure, and use 250 mL of deionized extract Dissolved in water, then extracted five times with equal volumes of petroleum ether and ethyl acetate, respectively. Take 500 g of AB-8 macroporous resin, put it into a chromatographic column with a diameter of 20 cm, load the aqueous phase, and elute with 30% and 50% ethanol in sequence. The 50% ethanol eluate was concentrated to dryness under reduced pressure and stored in the refrigerator for further HSCCC separation.

[0041] 2. Preparation of spermidine by high-speed countercurrent separation

[0042] Prepare a two-phase solvent system of chloroform-methanol-water (1:1:1, v / v) in a separatory funnel, shake well and let stand overnight. The ...

Embodiment 2

[0051] 1. Preparation of safflower spermidine crude extract

[0052] The preparation of the crude extract of safflower spermidine was the same as in Example 1.

[0053] 2. Preparation of spermidine by high-speed countercurrent separation

[0054] Prepare a two-phase solvent system of chloroform-methanol-water (4:5:4, 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.

[0055] Pump the lower phase of the solvent system into the main engine with a flow rate of 15 mL / min and fill the separation solenoid, turn on the circulating water bath and set the temperature to 25 °C. Turn on the power of the main engine and rotate it forward at 850 r / min. After the rotation speed is stable, pump ...

Embodiment 3

[0057] 1. Preparation of safflower spermidine crude extract

[0058] The preparation of the crude extract of safflower spermidine was the same as in Example 1.

[0059] 2. Preparation of spermidine by high-speed countercurrent separation

[0060] Prepare a two-phase solvent system of chloroform-methanol-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 120 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.

[0061]Pump the lower phase of the solvent system into the main engine with a flow rate of 15 mL / min and fill the separation solenoid, turn on the circulating water bath and set the temperature to 25 °C. Turn on the power of the main engine and rotate it forward at 850 r / min. After the rotation speed is stable, pump t...

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Abstract

The invention relates to a separation method of natural medicines, and specifically relates to a method for separation and preparation of spermidines from safflower by employing high-speed counter-current chromatography. The method comprises the following steps: (1) mixing chloroform, methanol and aqueous solution to form a mixed solvent, layering; (2) dissolving safflower spermidine crude extract in the lower layer of the mixed solvent obtained in the step (1); (3) layering the mixed solvent in the step (1) for obtain a solid phase and a mobile phase, injecting the solution in the step (2) into chromatographic column via an admission valve, continuously pumping the mobile phase after injection is finished; and (4) collecting isolates and concentrating to obtain first spermidine, a second spermidine, third spermidine and fourth spermidine. By employing the high-speed counter-current chromatography and the reasonable solvent system, high-purity spermidine compounds are extracted from safflower; on solid-phase carrier is needed, and no irreversible adsorption exists, spermidines are prepared efficiently rapidly with low cost and without sample loss and without pollution. The method is simple in technology, convenient to operate, safe, good in repeatability, and applicable to industrialized production.

Description

technical field [0001] The invention relates to a method for separating natural medicines, in particular to a method for separating and preparing four cis-trans isomers of spermidine from safflower by high-speed countercurrent chromatography. Background technique [0002] The dried flowers of safflower, a plant belonging to the family Compositae, can "promote blood circulation, moisten dryness, relieve pain, relieve swelling and stimulate menstruation". Traditional Chinese medicine believes that safflower is pungent, slightly bitter, warm in nature, returning to the heart and liver meridian. Diseases such as angina and high blood pressure. Safflower has become an important traditional Chinese medicine for the prevention and treatment of coronary heart disease, myocardial infarction and cerebral thrombosis in modern clinical practice. Modern pharmacological experiments show that safflower can improve the oxygen supply of heart and brain, reduce ischemic injury, anticoagulan...

Claims

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Application Information

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IPC IPC(8): C07C231/24C07C235/34
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
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