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Method for separating and purifying bergamot lactone from clausena dentata

A technology of bergamot lactone and tooth leaf yellow bark, applied in the field of chemistry, to achieve the effect of simple steps

Pending Publication Date: 2021-03-09
淮安市厚沐医疗技术咨询中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, it is still unknown whether high-speed countercurrent chromatography can be used to separate the bergamot lactone in P. serrata from other compounds contained in P. serrata to prepare high-purity bergamot lactone

Method used

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  • Method for separating and purifying bergamot lactone from clausena dentata
  • Method for separating and purifying bergamot lactone from clausena dentata
  • Method for separating and purifying bergamot lactone from clausena dentata

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Embodiment Construction

[0022] 1. Instruments and reagents

[0023] TBE-300B high-speed countercurrent chromatograph is a product of Shanghai Tongtian Biotechnology Co., Ltd.

[0024] Agilent-1260 high performance liquid chromatograph is a product of Agilent.

[0025] The chromatographic column Diamonsil C18 (250mm×4.6mm, 5μm) is a product of Dima Technology.

[0026] The organic solvents used in high-speed countercurrent are all conventional analytical pure solvents, the organic solvents used in high performance liquid chromatography are all conventional chromatographic pure solvents, and the water is deionized water.

[0027] The bergamot lactone reference substance was purchased from Shanghai Yuanye Biotechnology, with a purity of ≥98%.

[0028] 2. Methods and results

[0029] 1. Preparation of crude extract

[0030] Grind the dried branches and leaves of P. serrata through a 40-mesh sieve, add 90% ethanol aqueous solution according to the ratio of material to liquid 1kg / 5L, heat reflux for ex...

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Abstract

The invention discloses a method for separating and purifying bergamot lactone from clausena dentata. The method comprises the following steps: S1, preparation of an extract crude product: adding dried branches and leaves of clausena dentata into an ethanol aqueous solution for extraction, filtering, concentrating under reduced pressure to obtain extract, adding water into the extract for suspension, extracting with petroleum ether, and recovering the solvent to obtain an extract crude product, and S2, performing HSCCC separation on the crude extract: taking cyclohexane / ethyl acetate / n-butyl alcohol / methanol / water in a volume ratio of 6: 4: 1: 5: 5 as a solvent system, taking an upper phase as a stationary phase, taking a lower phase as a mobile phase, taking a host rotating speed as 850 r / min and a mobile phase flowing speed as 2 mL / min, after two phases are balanced, feeding a sample, starting to record a chromatogram at the same time, collecting 140min-165min eluent, and performingvacuum concentration until the eluent is dry. The method is simple in step, and the raw material advantages of the clausena lansium are fully utilized.

Description

technical field [0001] The invention belongs to the field of chemistry, and in particular relates to a method for separating and purifying bergamot lactone from the yellow bark of serrata. Background technique [0002] Bergamot lactone is a kind of coumarin compound, which widely exists in natural plants and has various pharmacological activities such as anticancer and analgesic. The chemical structure of bergamotide is as follows. [0003] [0004] Hu Lifeng et al. provided a method for the separation and purification of bergamot lactone in notopterygium by silica gel column chromatography-high-speed countercurrent chromatography (Separation and purification of bergamot lactone in notopterygium by silica gel column chromatography-high-speed countercurrent chromatography, Chinese Herbal Medicine, Volume 44, Issue 6 March 2013), but this method still needs to rely on the silica gel column chromatography that is loaded down with trivial details not easy to use in mass prod...

Claims

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Application Information

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IPC IPC(8): C07D493/04
CPCC07D493/04
Inventor 洪其昌
Owner 淮安市厚沐医疗技术咨询中心
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