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A kind of separation and purification method of isopyrheum lactone monomer

A technology for separation and purification of isoviolet foregone lactone, which is applied in chemical instruments and methods, organic chemistry, chemical recovery and other directions, can solve the problems of low content of lactones, strict requirements on process parameters, and inability to meet market needs, and the like, To achieve the effect of low toxicity, stable process and convenient product quality

Active Publication Date: 2019-03-29
CHENGDU PUSH BIOLOGICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this technical scheme has complicated process and strict requirements on process parameters. At the same time, the isolated lactones have low content and low purity, which cannot meet the needs of the market; Isomers of the target compound isomers of proscaractin, and it is a chiral isomer
Separation and purification of chiral isomers by traditional methods is extremely difficult, costly, and monomer purity is low

Method used

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  • A kind of separation and purification method of isopyrheum lactone monomer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] A method for isolating and purifying P. chinensis Lactone monomer, comprising the following process steps:

[0046] A. to extract

[0047] Weigh 5Kg of notopterygium rhizome, crush it into a coarse powder of 1-4 mm, add 10 L of ethanol solution with a volume concentration of 95%, extract 3 times, 2 hours each time, recover ethanol, and combine the extracts, a total of 2.9 L, which is the extract Ⅰ ;

[0048] B. Extraction

[0049] Add an equal volume of ethyl acetate to the extract I obtained in step A, extract 3 times, remove the aqueous solution in the lower layer, recover the residual ethyl acetate, and obtain a total of 1.8 L of concentrated solution to obtain extract II;

[0050] C. Macroporous resin column chromatography

[0051] 1.8 L of the extract II obtained in step B was enriched with an activated macroporous resin column. After the enrichment was completed, it was washed with 10 L of deionized water and analyzed with 15 L of ethanol with a volume concentr...

Embodiment 2

[0065] A method for isolating and purifying P. chinensis Lactone monomer, comprising the following process steps:

[0066] A. to extract

[0067] Weigh 50Kg of notopterygium rhizome, crush it into a coarse powder of 1-4 mm, add 110 L of ethanol solution with a volume concentration of 95%, extract 3 times, 2 hours each time, recover the ethanol, and combine the extracts, a total of 30 L, which is the extract Ⅰ;

[0068] B. Extraction

[0069] Add an equal volume of ethyl acetate to the extract I obtained in step A, extract 3 times, remove the aqueous solution in the lower layer, recover the residual ethyl acetate, and obtain a total of 20 L of the concentrated solution to obtain the extract II;

[0070] C. Macroporous resin column chromatography

[0071] 20L of the extract II obtained in step B was enriched with an activated macroporous resin column. After the enrichment was completed, it was washed with 80L of deionized water and analyzed with 100L of ethanol with a volume c...

Embodiment 3

[0085] A method for isolating and purifying P. chinensis Lactone monomer, comprising the following process steps:

[0086] A. to extract

[0087] Weigh 100Kg of notopterygium rhizome, crush it into a coarse powder of 1-4 mm, add 250 L of ethanol solution with a volume concentration of 95%, extract 4 times, 3 hours each time, recover ethanol, and combine the extracts, a total of 70 L, which is the extract Ⅰ;

[0088] B. Extraction

[0089] Add an equal volume of ethyl acetate to the extract I obtained in step A, extract 3 times, remove the aqueous solution in the lower layer, recover the residual ethyl acetate, and obtain a total of 50 L of concentrated solution to obtain extract II;

[0090] C. Macroporous resin column chromatography

[0091] 50L of the extract II obtained in step B was enriched with an activated macroporous resin column. After the enrichment was completed, it was washed with 100L of deionized water and analyzed with 150L of ethanol with a volume concentrati...

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Abstract

The invention relates to a separation purification method of a marmesin monomer, belonging to the technical field of extraction of traditional Chinese medicine compounds. The method comprises the following steps: by using umbelliferae notopterygium root as the raw material, carrying out ethanol solution extraction, ethyl acetate extraction, macroporous resin column chromatography, silica gel column chromatography, high-performance preparative liquid chromatography separation and acid hydrolysis to obtain the marmesin monomer. By using the proper technique and parameter conditions, the marmesin content in the product reaches 99% or above. The whole technical process is stable, is simple to operate, has the advantages of high separation efficiency and low cost, and can perform mass high-purity separation to prepare the marmesin monomer.

Description

technical field [0001] The invention relates to a method for preparing a plant compound monomer, in particular to a method for separating and purifying a plant compound monomer, and belongs to the technical field of separation and purification of a traditional Chinese medicine compound monomer. Background technique [0002] Notopterygium (Rhizoma et Radix Notopterygii) is the dried rhizome and root of Notopterygium incisum Ting ex H. T. Chang or Notopterygium forbesii Boiss. of Umbelliferae. Notopterygium is warm in taste, bitter and pungent, enters the bladder and kidney meridian, has the effect of dispelling exterior cold, removing rheumatism, and sharpening joints, and can treat exogenous wind-cold, headache without sweating, wind-cold-damp arthralgia, strong neck and tendons, aching joints, feng shui edema, pain Sores, etc. [0003] The English name of different purple flower Peucedanum lactone is Marmesin, and its molecular formula is C 14 h 14 o 4 , the molecular w...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D493/04C07H15/26C07H1/00
CPCY02P20/582
Inventor 李波文焕松吴涛李启发刘丁
Owner CHENGDU PUSH BIOLOGICAL TECH