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Method for purifying glaucocalyxin A

A purification method, the technology of cyanine A, which is applied in the field of natural medicinal chemistry, can solve the problems of cumbersome methods, long purification cycle, and low yield, and achieve the effect of solving low separation yield and overcoming the small amount of liquid phase treatment

Inactive Publication Date: 2013-01-02
NANJING ZELANG AGRI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As mentioned above, the existing methods for purifying cyanine A have long purification period, low yield and cumbersome methods.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Extraction: Grind the whole plant of Lemonia sativa, pass through a 60-mesh sieve, take 500g and put it into the extraction kettle, and pass it into supercritical CO 2 For extraction, set the parameters of the extraction kettle: the extraction temperature is 35°C, the pressure is 25MPa, and CO 2 The flow rate is 20L / h. After the environment in the extraction tank is stabilized, ethyl acetate is introduced as an entrainer. The flow rate is 500ml / h, and the extraction is performed for 3 hours.

[0016] Purification: Take n-hexane, ethyl acetate, methanol, and water, and mix them according to 1:3:2:3. After fully layering, take the upper phase and inject it into a high-speed countercurrent chromatography tube as a stationary phase. Turn on the main engine at a speed of 700rpm. Pump into the lower phase as the stationary phase. After the dynamic equilibrium is established, the flow rate is adjusted to 2ml / min. The extract is dissolved with the mobile phase, and the sample i...

Embodiment 2

[0018] Extraction: Grind the whole plant of Leucaphylla saponica, pass through a 80-mesh sieve, take 500g and put it into the extraction kettle, and pass it into the supercritical state of CO 2 For extraction, set the parameters of the extraction kettle: the extraction temperature is 45°C, the pressure is 30MPa, and CO 2 The flow rate is 25L / h. After the environment in the extraction tank is stabilized, ethyl acetate is introduced as an entrainer. The flow rate is 500ml / h, and the extraction is performed for 2 hours.

[0019] Purification: Take n-hexane, ethyl acetate, methanol, and water, and mix them according to 2:5:4:5. After fully layering, take the upper phase and inject it into a high-speed countercurrent chromatographic tube as a stationary phase. Turn on the main engine at a speed of 800 rpm. Pump into the lower phase as the stationary phase. After the dynamic equilibrium is established, the flow rate is adjusted to 3ml / min. The extract is dissolved with the mobile ph...

Embodiment 3

[0021] Extraction: Grind the whole plant of Leucaphyllum saponica, pass through a 40-mesh sieve, take 500g and put it into the extraction kettle, and pass it into supercritical CO 2 For extraction, set the parameters of the extraction kettle: the extraction temperature is 40°C, the pressure is 27MPa, and CO 2 The flow rate is 22L / h. After the environment in the extraction tank is stabilized, ethyl acetate is introduced as an entrainer. The flow rate is 400ml / h, and the extraction is performed for 3 hours.

[0022] Purification: Take n-hexane, ethyl acetate, methanol, and water, and mix them according to 3:10:5:7. After fully layering, take the upper phase and inject it into a high-speed countercurrent chromatographic tube as a stationary phase. Pump into the lower phase as the stationary phase. After the dynamic equilibrium is established, the flow rate is adjusted to 1ml / min. The extract is dissolved with the mobile phase, and the sample is injected by the injection valve. Th...

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PUM

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Abstract

The invention discloses a method for purifying glaucocalyxin A. The method includes using rabdosia japonica as a raw material, smashing the rabdosia japonica, enabling the smashed rabdosia japonica to pass through a sieve with 20 meshes to 80 meshes, then throwing the rabdosia japonica into an extraction kettle, feeding liquid CO2 and cosolvents to perform supercritical extraction to obtain an extract, purifying the extract by a high-speed counter-current chromatography, using an ultraviolet detector for on-line monitoring, collecting target components, recycling reagents, and drying to obtain the purified glaucocalyxin A. The method has the advantages of being efficient, rapid, environment-friendly and capable of being popularized and used in an industrialized mode.

Description

technical field [0001] The invention belongs to the field of natural medicine chemistry, and in particular relates to a method for purifying schicin A. Background technique [0002] Glaucocalyxin A is a kaurene-type diterpenoid, CAS number: 79498-31-0, molecular formula C 20 h 28 o 4 , molecular weight 332.43, molecular structure: [0003] . [0004] Blue Calyx Fragrant Chacai is a plant of the genus Lamiaceae, also known as Fragrant Chacai, Shansuzi, Huicaihua, and Daogenyesu. The whole herb is used as medicine, which has the effects of clearing away heat, dehumidification and detoxification. It is used for colds, sore throat, tonsillitis, gastritis, hepatitis, mastitis, cancer (esophageal cancer, cardia cancer, liver cancer, breast cancer). [0005] Now studies have found that the blue calyx calyx contains a large amount of diterpenoids, mainly the blue calyxin A, which has significant cytotoxic activity. [0006] The purification method of cyanine A generally adop...

Claims

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Application Information

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IPC IPC(8): C07C49/743C07C45/78
CPCY02P20/141Y02P20/54
Inventor 苏刘花
Owner NANJING ZELANG AGRI DEV
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