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Method for preparing lobetyolin, atractylenolide III and syringin from codonopsis pilosula based on PRE-HPLC

A technology of tangshenoside and atractylodes lactone, which is applied in chemical instruments and methods, preparation of sugar derivatives, and resistance to vector-borne diseases, etc., can solve the problems of large consumption of reagents, cumbersome process steps, and single separation components, and achieve The effect of improving efficiency, simple process and high product purity

Active Publication Date: 2021-08-10
JING BRAND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, the extraction and separation methods for obtaining these functional components from Codonopsis Codonopsis medicinal materials: generally use countercurrent extraction, ultrasonic extraction, extraction, etc., or modify the target components in a certain way and then further separate them. Separation and purification are carried out in a combination of low-pressure preparation, and high-purity monomer compounds are also obtained through supercritical fluid extraction and other methods. However, most of these methods have cumbersome process steps, consume a large amount of reagents, and the monomer yield is relatively Low, and only 1-2 kinds of monomer components can be obtained each time. If multiple monomer components need to be obtained, it is necessary to adopt different conditions or methods for multiple operations. Therefore, it generally has a long cycle, complex process, and high efficiency. Disadvantages such as low cost, high cost, and single separation component

Method used

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  • Method for preparing lobetyolin, atractylenolide III and syringin from codonopsis pilosula based on PRE-HPLC
  • Method for preparing lobetyolin, atractylenolide III and syringin from codonopsis pilosula based on PRE-HPLC
  • Method for preparing lobetyolin, atractylenolide III and syringin from codonopsis pilosula based on PRE-HPLC

Examples

Experimental program
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Effect test

Embodiment 1

[0028] A method for preparing tangshenoside, atractyllide III and syringin from Radix Codonopsis based on PRE-HPLC, comprising the following steps:

[0029] (1) Medicinal material extraction: Take 100 g of Codonopsis pilosula, crush it, add 12 times the volume of 65% ethanol solution, 1200 mL each time, 400 W ultrasonic extraction for 60 min, and extract 3 times in total. After the extraction, coarse filter, collect and combine the filtrates.

[0030] (2) Concentration and drying: the above extract was concentrated and dried under reduced pressure at 45° C. to obtain 9.9 g of Codonopsis pilosula crude extract.

[0031] (3) Preparation and purification: take an appropriate amount of dried Codonopsis pilosula extract and add 100 times the amount of 70% ethanol solution to ultrasonically dissolve, then pass through a 0.22 μm microporous membrane to obtain the sample to be prepared, and finally separate and prepare by preparing the liquid phase, chromatographic conditions For: the...

Embodiment 2

[0037] A method for preparing tangshenoside, atractyllide III and syringin from Radix Codonopsis based on PRE-HPLC, comprising the following steps:

[0038] (1) Medicinal material extraction: Take 100 g of Codonopsis pilosula, crush it, add 14 times the volume of 70% ethanol solution, 1400 mL each time, 450W ultrasonic extraction for 45 min, and extract 3 times in total. After the extraction, coarse filter, collect and combine the filtrates.

[0039] (2) Concentration and drying: the above extract was concentrated and dried under reduced pressure at 60° C. to obtain 10.4 g of Codonopsis pilosula crude extract.

[0040] (3) Preparation and purification: take an appropriate amount of dried Codonopsis pilosula extract and add 150 times the amount of 65% ethanol solution to ultrasonically dissolve, then pass through a 0.22 μm microporous membrane to obtain the sample to be prepared, and finally separate and prepare by preparing the liquid phase, chromatographic conditions For: the...

Embodiment 3

[0046] A method for preparing tangshenoside, atractyllide III and syringin from Radix Codonopsis based on PRE-HPLC, comprising the following steps:

[0047] (1) Medicinal material extraction: Take 100 g of Codonopsis pilosula, crush it, add 15 times the volume of 75% ethanol solution, 1500 mL each time, 500 W ultrasonic extraction for 60 min, and extract 3 times in total. After the extraction, coarse filter, collect and combine the filtrates.

[0048] (2) Concentration and drying: the above extract was concentrated and dried under reduced pressure at 50° C. to obtain 10.7 g of Codonopsis pilosula crude extract.

[0049] (3) Preparation and purification: take an appropriate amount of dried Codonopsis pilosula extract and add 200 times the amount of 75% ethanol solution to ultrasonically dissolve, then pass through a 0.22 μm microporous membrane to obtain the sample to be prepared, and finally separate and prepare by preparing the liquid phase, chromatographic conditions For: th...

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Abstract

The invention discloses a method for preparing lobetyolin, atractylenolide III and syringin from codonopsis pilosula based on PRE-HPLC, and the method specifically comprises the following steps: (1) single medicine extraction: taking a codonopsis pilosula medicinal material, crushing, adding 12-15 times of ethanol solution, carrying out ultrasonic extraction at 400-500W for 2-3 times, each time for 30-60min, after the extraction is finished, carrying out rough filtration, and mixing filtrate to obtain a codonopsis pilosula extracting solution; (2) concentrating and drying: performing reduced-pressure vacuum concentration and drying on the filtered extracting solution; (3) preparing and purifying: ultrasonically dissolving the dried extract, filtering through a 0.22 mu m microporous filter membrane, and preparing a liquid phase; (4) fraction collection: respectively collecting lobetyolin, atractylenolide III and syringin fractions; and (5) concentrating and drying: concentrating and drying the collected fractions under reduced pressure in vacuum. The method has the characteristics of convenience in operation, good reproducibility, short period, simultaneous preparation of three monomer components and the like, and the prepared monomer components have the characteristic of high purity.

Description

technical field [0001] The invention relates to the technical field of separation and purification of chemical components, in particular to a method for rapidly separating and preparing tangshenoside, atractylide III and syringin from Codonopsis pilosula extract based on high-efficiency preparative liquid chromatography. Background technique [0002] Codonopsis pilosula (Codonopsis pilosula (Franch.) Nannf.), Codonopsis pilosula Nannf.var.modesta (Nannf.) L.T.Shen) or Codonopsis pilosula (Codonopsistangshen Oliv.) dry roots and rhizomes of Codonopsis pilosula (Franch.) Nannf. The name of Codonopsis Codonopsis first appeared in "Materia Medica Congxin", which said: "According to the ancient Materia Medica cloud: the ginseng must go to the party is the best. The herbal medicines of the past dynasties are included, and they are commonly used Chinese herbal medicines in the Chinese Pharmacopoeia. They are excavated in autumn, washed and dried. This book Sweet in taste, flat in n...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/203C07H1/08C07D307/92
CPCC07H15/203C07H1/08C07D307/92Y02A50/30
Inventor 陈志超徐剑杨跃军石万银
Owner JING BRAND
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