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Method for extracting caragana microphylla from hypaphorine

A technology of Erythrina haipa and Caragana lobularis is applied in the biological field, which can solve the problems of large amount of solvent, low extraction efficiency, complicated operation and the like, and achieves the effects of no sample loss, continuous preparation and reduction of environmental pollution.

Inactive Publication Date: 2013-01-30
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Traditional extraction methods have disadvantages such as low extraction efficiency, small output, complicated operation, large amount of solvent and serious pollution.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The raw material of Caragana microphylla is crushed, passed through a 40-mesh sieve, and 1kg is put into the extraction kettle, and the liquid CO is introduced under the conditions of extraction pressure 23MPa and temperature 45℃ 2 , Flow rate 20kg / h, while passing 80% methanol solution as entrainer, dynamic extraction for 40min, analysis under pressure 5MPa, temperature 50℃, the obtained extract is dissolved in acid water, filtered to adjust pH5, added ethanol and alcohol precipitation, filtered Get the precipitate. Mix n-hexane, ethyl acetate, methanol, and water in a ratio of 1:3:4:5. After fully layering, take the upper phase and fill the high-speed countercurrent chromatographic column. At the same time, turn on the host at 800 rpm, and pump the lower phase as the mobile phase. After the system is equilibrated, the flow rate is adjusted to 3ml / min. At the same time, the sediment is dissolved with the mobile phase, and the sample is injected by the injection valve, mo...

Embodiment 2

[0022] The raw material of Caragana microphylla is crushed, passed through an 80-mesh sieve, and 1kg is put into the extraction kettle, and the liquid CO is introduced under the conditions of extraction pressure 30MPa and temperature 35℃ 2 , The flow rate is 22kg / h, and 90% methanol solution is introduced as the entrainer at the same time. The dynamic extraction is carried out for 40 minutes, and the solution is analyzed at a pressure of 5MPa and a temperature of 50°C. The obtained extract is dissolved in acid water, filtered to adjust pH5 and added ethanol and alcohol precipitation, filtered Get the precipitate. Take n-hexane, ethyl acetate, methanol, and water and mix 1:5:4:9. After fully stratifying, take the upper phase and fill the high-speed countercurrent chromatographic column. At the same time, turn on the host at 800rpm, and pump the lower phase as the mobile phase. After the system is equilibrated, the flow rate is adjusted to 1ml / min, while the sediment is dissolved ...

Embodiment 3

[0024] The raw material of Caragana microphylla was crushed, passed through a 60-mesh sieve, and 1 kg was put into the extraction kettle. Under the conditions of extraction pressure of 25MPa and temperature of 40°C, liquid CO was introduced. 2 At the same time, the flow rate is 25kg / h, and 60% methanol solution is introduced as the entrainer. The dynamic extraction is performed for 50 minutes, and the solution is analyzed at a pressure of 6MPa and a temperature of 60°C. The obtained extract is dissolved in acid water, filtered and adjusted to pH 5-6 and added with ethanol for precipitation. The precipitate was filtered. Take n-hexane, ethyl acetate, methanol, and water and mix 2:5:5:6. After fully layering, take the upper phase and fill the high-speed countercurrent chromatographic column. At the same time, turn on the host at 900rpm, and pump the lower phase as the mobile phase. After the system is equilibrated, the flow rate is adjusted to 2ml / min. At the same time, the sedime...

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Abstract

The invention discloses a method for extracting caragana microphylla from hypaphorine with high efficiency. The method comprises the following steps of: grinding a caragana microphylla raw material into powder with the granular diameter of 20 to 80 meshes, extracting by using supercritical CO2, introducing an entrainer, extracting for 30 to 60min, resolving under a pressure of 5 to 9MPa and at 40 to 60 DEG C to obtain the extract; and dissolving the extract in acid water, filtering, regulating the pH value to 5 to 6, precipitating in ethanol, carrying out high-speed counter-current chromatography of the precipitate, detecting the precipitate on line in an ultraviolet detector, collecting target fractions, and drying under reduced pressure to obtain hypaphorine. The method, when used in production, can increase extraction efficiency and simplify purification steps and is environment-friendly.

Description

technical field [0001] The invention belongs to the field of biotechnology, and in particular relates to a method for extracting hepatine from Caragana microphylla. Background technique [0002] Hypaphorine, also known as Hypaphorine, CAS number: 487-58-1, molecular formula: C 14 o 18 N 2 o 2 , molecular weight 246.3, molecular structure: [0003] . [0004] The results of the study showed that erythraline can significantly inhibit the ear swelling of mice, reduce the weight of the ear pinna of mice; increase the weight of thymus and spleen of mice, increase the level of serum hemolysin in mice; significantly reduce the levels of CCL4 and naphthalene isothiocyanate Ester-induced liver injury mice serum transaminase activity and bilirubin content, protect liver injury. [0005] Caragana microphylla is a plant of the leguminous family Rosaceae. Its fruit, flower, and root are used in traditional Chinese medicine. The fruit of traditional Chinese medicine: bitter in tas...

Claims

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Application Information

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IPC IPC(8): C07D209/20
CPCY02P20/54
Inventor 刘东锋杨成东
Owner NANJING ZELANG MEDICAL TECH
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