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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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Problems solved by technology

However, the inventors have found that there is no report of using HSCCC to separate and purify various amides from Piperaceae

Method used

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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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preparation example Construction

[0023] In a typical embodiment of the present invention, a kind of efficient preparation method of high-purity amide alkaloid component is provided, and described preparation method comprises at least:

[0024] The total extract of Piperamide alkaloids was dissolved in a solvent system, and high-speed countercurrent chromatography was used for one-dimensional countercurrent chromatography to obtain two kinds of Piperamide alkaloids; The blowing part is separated by off-line two-dimensional gradient countercurrent chromatography using high-speed countercurrent chromatography to obtain eight kinds of Piperamide alkaloids; the solvent system in the separation and extraction method is n-hexane / ethyl acetate / methanol / water.

[0025] In yet another specific embodiment of the present invention, the preparation method of the total extract of Piperaceae amide alkaloids is as follows: take Piperaceae and pulverize them, add ethanol to reflux for extraction, concentrate, adjust the pH to ...

Embodiment

[0041] 1. Sample Extraction

[0042] Take 1.8 kg of dried Piperumba, grind and sieve it with a pulverizer, use 95% ethanol at a ratio of 1:10 solid to liquid, extract under reflux at 85°C for 3 hours, and repeat the operation three times. The extracts were combined, concentrated by suction filtration, and distilled water was added to obtain 250 mL of a crude extraction solution. The pH was adjusted to 2 by adding hydrochloric acid, and extracted three times with an equal volume of petroleum ether. Ammonium hydroxide was added to the remaining aqueous phase to adjust the pH to 9, extracted three times with 250 mL of chloroform, the combined filtrates were concentrated under reduced pressure to obtain 113 g of the chloroform phase, and the sample extraction rate was 6.2%. The samples were stored in a refrigerator at 4°C.

[0043] 2. One-dimensional countercurrent chromatographic separation of total extracts

[0044] The solvent system in high-speed countercurrent chromatography...

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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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