阅读说明：本技术 一种高效制备穿心莲内酯的方法 (Method for efficiently preparing andrographolide ) 是由 杨成东 于 2018-05-30 设计创作，主要内容包括：本发明公开了一种高效制备穿心莲内酯的方法。方法步骤如下：A取穿心莲粗粉,加入超临界CO2萃取釜,设置温度40~65℃、压力20~40MPa,通入液态CO2,流量为20~50L/h,萃取时间30~200min,解析得萃取物；B上述萃取物用乙醇溶液溶解,加入活性炭回流脱色,脱色液浓缩后用乙酸乙酯萃取,萃取液浓缩结晶,结晶物再用乙醇溶解,采用高速逆流色谱法分离,根据色谱收集流分,减压浓缩干燥即得。采用本方法制备穿心莲内酯,制备工艺简单,污染小,易于实现工业化生产。(The invention discloses a method for efficiently preparing andrographolide, which comprises the following steps of A, taking coarse andrographis paniculata powder, adding the coarse andrographis paniculata powder into a supercritical CO2 extraction kettle, setting the temperature to be 40 ~ 65 ℃ and the pressure to be 20 ~ 40MPa, introducing liquid CO2, enabling the flow rate to be 20 ~ 50L/h, enabling the extraction time to be 30 ~ 200min, resolving to obtain an extract, B, dissolving the extract with an ethanol solution, adding active carbon, carrying out reflux decoloration, concentrating a decolored solution, extracting with ethyl acetate, concentrating and crystallizing an extract, dissolving a crystal with ethanol, separating by adopting a high-speed counter-current chromatography, collecting fractions according to chromatography, and carrying out reduced pressure concentration and drying.)

1. a method for efficiently preparing andrographolide is characterized by comprising the following steps:

A, adding coarse powder of common andrographis herb into a supercritical CO2 extraction kettle, setting the temperature at 40 ~ 65 ℃ and the pressure at 20 ~ 40MPa, introducing liquid CO2, controlling the flow at 20 ~ 50L/h and the extraction time at 30 ~ 200min, and resolving to obtain an extract;

And B, dissolving the extract with an ethanol solution, adding activated carbon, refluxing and decoloring, concentrating the decolored solution, extracting with ethyl acetate, concentrating and crystallizing the extract, dissolving the crystal with ethanol, separating by adopting a high-speed counter-current chromatography, collecting fractions according to the chromatography, concentrating under reduced pressure and drying to obtain the compound.

2. the method of claim 1, wherein the high-speed countercurrent chromatography separation in step B is performed by mixing acetonitrile, methanol, and disodium hydrogen phosphate solution (ph 6.2) as solvent system at a ratio of 2-4:1-5:4-7, and collecting the upper phase as stationary phase and the lower phase as mobile phase.

Technical Field

The invention belongs to the technical field of biology, and particularly relates to a method for preparing andrographolide.

Background

The herba Andrographitis is herb or leaf of Andrographis paniculata (Burmf) Ness) belonging to Acanthaceae. Andrographis paniculata contains various diterpenoid compounds, mainly including andrographolide (andrographolide), dehydroandrographolide (andrographolide), deoxyandrographolide (andrographolide), neoandrographolide (andrographolide), high andrographolide, etc. Wherein, the main components of the antibacterial and anti-inflammatory agent are andrographolide and neoandrographolide. The whole herb of common andrographis herb can be used as a medicine, has the effects of clearing heat and removing toxicity, diminishing inflammation, cooling blood and stopping swelling, is widely applied to the treatment of gastroenteritis, pneumonia, otitis media, bronchitis, dysentery, sphagitis, traumatic infection, water and fire scald, snake venom bite, urinary tract infection, wind-heat type common cold, tonsillitis and the like, is known as a natural spectrum antibiotic medicine, and is widely applied clinically.

The existing methods for preparing andrographolide are mostly extracted by conventional organic reagents such as ethanol and the like through literature retrieval, and the extraction method has low extraction efficiency and serious pollution and does not meet the requirement of environmental protection.

disclosure of Invention

The invention aims to overcome the defects of the prior art and provide an efficient and environment-friendly method for preparing andrographolide.

In order to solve the technical problems, the invention adopts the following technical scheme:

A method for preparing andrographolide is characterized by comprising the following steps:

A, adding coarse powder of common andrographis herb into a supercritical CO2 extraction kettle, setting the temperature at 40 ~ 65 ℃ and the pressure at 20 ~ 40MPa, introducing liquid CO2, controlling the flow at 20 ~ 50L/h and the extraction time at 30 ~ 200min, and resolving to obtain an extract;

And B, dissolving the extract with an ethanol solution, adding activated carbon, refluxing and decoloring, concentrating the decolored solution, extracting with ethyl acetate, concentrating and crystallizing the extract, dissolving the crystal with ethanol, separating by adopting a high-speed counter-current chromatography, collecting fractions according to the chromatography, concentrating under reduced pressure and drying to obtain the compound.

And B, performing high-speed countercurrent chromatographic separation in the step B, wherein acetonitrile, methanol and a disodium hydrogen phosphate solution (pH 6.2) are used as a solvent system, the solvent system is mixed according to the ratio of 2-4:1-5:4-7, the upper phase is taken as a stationary phase, and the lower phase is taken as a mobile phase.

The method has the advantages of high extraction efficiency, simple operation of the whole process, high product yield and easy realization of industrial production by adopting supercritical CO2 for extraction.

the present invention will be further described with reference to specific embodiments, but the scope of the invention as claimed is not limited to the following embodiments.

Detailed Description