Efficient preparation method and application of high-purity amide alkaloid component

A technology for high-purity amides and alkaloids, which is applied in the field of efficient preparation of high-purity amides and alkaloids, achieving the effects of good separation, simple preparation methods, and high purity

Active Publication Date: 2020-12-01
SHANDONG UNIV
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  • Efficient preparation method and application of high-purity amide alkaloid component
  • Efficient preparation method and application of high-purity amide alkaloid component
  • Efficient preparation method and application of high-purity amide alkaloid component

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[0023] An exemplary embodiment of the present invention, there is provided a high-purity amides alkaloids efficient production method, the production method comprising at least:

[0024] The Piper longum amide total alkaloids extract was dissolved in a solvent system, a high-speed countercurrent chromatography dimensional separation countercurrent chromatography to obtain two Piper longum amides alkaloids; non-separation column eluted remaining ingredients, i.e., the tail blow-off portion is a two-dimensional gradient countercurrent chromatography to obtain eight kinds of Piper longum amide alkaloid using high speed countercurrent chromatography; the separation and extraction process on the solvent system hexane / ethyl acetate / methanol / water.

[0025] Another specific embodiment of the present invention, a method for preparing Piper longum amides total alkaloid extract is: take Piper longum pulverized, add ethanol extracted, concentrated, water was added the pH was adjusted t...

Example Embodiment

[0040] Example

[0041] Sample extraction

[0042] The drying of 1.8 kg was dried, and the sieve was grinded with a pulverizer, and 95% ethanol was used to reflex 3 h at 85 ° C for 3 h, and the operation was repeated three times. The extract was combined, and the filtration was concentrated, and the distilled water was added to obtain 250 ml of a crude suction solution, and the hydrochloric acid was adjusted to 2, extracted 3 times with an equal volume petroleum ether. The residual aqueous phase was added to 9, extracted 3 times with 250 ml of chloroform, and concentrated under reduced pressure, and the sample extraction rate was 6.2%, and the sample was stored in a 4 ° C refrigerator.

[0043] 2. One-dimensional countercurrent spectrum separation of total extract

[0044] The solvent system in the high-speed countercurrent chromatography is n-hexane-ethyl acetate-methanol-water = 5: 4: 5: 4 (v / v), select the upper phase solution as a fixed phase, the lower phase solution is a ...

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Abstract

The invention provides an efficient preparation method and application of a high-purity amide alkaloid component, and belongs to the technical field of extraction and preparation of effective components of traditional Chinese medicines. According to the method, the total amide alkaloids in the piper longum are enriched through the pH value, therefore, the method for separating and purifying piperlongum amide alkaloids by high-speed counter-current chromatography is established. Finally, ten amide alkaloids such as piper longum minine are separated from the piper longum crude extract. The method lays a foundation for further research on pharmacological properties of piper longum amide alkaloid, research and development of related drugs and the like, is simple in separation and extraction method, good in separation degree and high in purity, has universality, and provides a new solution idea for extraction and analysis of alkaloid and other related compounds in piper longum and piper nigrum plants.

Description

technical field [0001] The invention belongs to the technical field of extraction and preparation of effective components of traditional Chinese medicines, and in particular relates to a high-efficiency preparation method and application of high-purity amide alkaloid components. Background technique [0002] The information disclosed in this background section is only intended to increase the understanding of the general background of the present invention, and is not necessarily taken as an acknowledgment or any form of suggestion that the information constitutes the prior art already known to those skilled in the art. [0003] Piper Longum (Piper Longum L.) is a representative plant of the genus Piper. It has a specific aroma, a spicy taste, and a flavor-enhancing effect. It is widely used in food processing such as roasting, roasting, and stewing. It is also one of the important spices one. Piper bark has a wide range of pharmacological effects. Piper bark can be used to...

Claims

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Application Information

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IPC IPC(8): C07D317/60C07C231/24C07C233/09
CPCC07C231/24C07D317/60C07C233/09
Inventor 孙蓉王岱杰李晓骄阳施树云刘闰平崔莉吕其刚黄娜娜吴东进邝江莹鹿庆华叶兰
Owner SHANDONG UNIV
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