A process for separating and purifying atractylolide i and atractylolide ii in Codonopsis pilosula with macroporous adsorption resin

A technology for separation of atractylolide and resin, which is applied in the field of natural medicinal chemistry, and can solve the problems of low extract content, low content of atractylide II, difficulty in enrichment, separation and purification, etc.

Active Publication Date: 2018-07-27
GANSU UNIV OF CHINESE MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The technical problem to be solved by the present invention is: the content of atractylolide I and atractylolide II in Codonopsis pilosula is relatively low, and there are certain difficulties in enrichment, separation and purification, especially atractylolide II, because the content in the extract is too low undetectable

Method used

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  • A process for separating and purifying atractylolide i and atractylolide ii in Codonopsis pilosula with macroporous adsorption resin
  • A process for separating and purifying atractylolide i and atractylolide ii in Codonopsis pilosula with macroporous adsorption resin
  • A process for separating and purifying atractylolide i and atractylolide ii in Codonopsis pilosula with macroporous adsorption resin

Examples

Experimental program
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Effect test

preparation example Construction

[0042] Preparation of reference solution

[0043] Accurately weigh 1.07 mg of the reference substance atractylide I and 1.12 mg of atractylide II, put them in a 10 mL volumetric flask, dissolve them with methanol and dilute to the mark, and shake well to obtain the reference substance 1. Draw up 1mL of reference substance 1 respectively, put it in a 100mL volumetric flask, dissolve it with methanol and dilute to the mark, and shake well to obtain reference substance 2.

[0044] Assay method

[0045] Chromatographic conditions: Chromatographic column: Thermo ODS HYPERSIL column; detection wavelength: 277nm for atractylolide I, 220 nm for atractylolide II; column temperature: 25°C; flow rate: 1mL / min; mobile phase: acetonitrile (B)-water (A); Gradient elution: 0 ~13min, 25%B; 13~35min, 60%B; 35~40min, 100%B; 40~55min, 100%B; injection volume: 20µL.

[0046] Optimization of Chromatographic Conditions

[0047]Selection of detection wavelength: select the absorption waveleng...

Embodiment 1

[0050] Example 1 Preparation of Codonopsis Codonopsis Crude Extract

[0051] Mix Codonopsis 95% ethanol at a weight ratio of 1:5, heat up to reflux for extraction for 2 hours, filter after completion, and concentrate the filtrate to dryness under reduced pressure. The solid is Codonopsis crude extract, which can be prepared by adding water to obtain extract solutions of different concentrations.

Embodiment 2

[0052] The selection of embodiment 2 macroporous adsorption resin types

[0053] The Codonopsis crude extract and water in Example 1 were prepared according to the weight / volume ratio of 0.125 g / mL to obtain an extract solution.

[0054] Weigh 1.00 g of 5 kinds of macroporous resins D101, HPD-100, H103, DM130, and S-8 that have been processed, put them into conical flasks with stoppers, add 30 mL of extract solution to each, place on a shaker and shake for 24 h, taken out, suction filtered, and the filtrate was treated for content determination. Add 50 mL of 95% ethanol solution to the resin, shake it on a shaker for 24 hours, take it out, filter it with suction, and measure the content of the filtrate as a desorption liquid after treatment. Calculate the adsorption amount, desorption amount, desorption rate and dry Solid quantity.

[0055] The calculation formulas of macroporous resin adsorption capacity, adsorption rate, desorption capacity and desorption rate are as follo...

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Abstract

The invention relates to a technology for separating and purifying atractylenolide I and atractylenolide II in radix codonopsis by using macroporous adsorption resin, belonging to the technical field of natural pharmaceutical chemistry. The technology comprises the following steps: 1, extracting the radix codonopsis by using an alcohol solution to obtain alcohol extract; carrying out vacuum concentration on the alcohol extract to dry, wherein the obtained solid is an extract of the radix codonopsis, and adding water into the solid for dissolving so as to obtain an extract solution; 2, absorbing the extract solution by using the macroporous adsorption resin DM130, and then desorbing by using the alcohol solution to obtain a desorbed solution; 3, carrying out vacuum concentration on the desorbed solution to dry so as to obtain an extract containing the atractylenolide I and the atractylenolide II. By utilizing the macroporous adsorption resin DM130 to separate and purify the atractylenolide I and the atractylenolide II in the radix codonopsis, the technology has the characteristics of being rapid in absorption speed, high in desorption rate, large in absorption capacity, high in elution rate, and the like, and the product is stable in desorption rate, so that the technology provided by the invention is an effective technology for deep utilization of the radix codonopsis.

Description

technical field [0001] The invention relates to a process for separating and purifying atractylide I and atractylide II in Codonopsis pilosula with macroporous adsorption resin, and belongs to the technical field of natural medicine chemistry. Background technique [0002] The traditional Chinese medicine Codonopsis Codonopsis is derived from three varieties of Platycodonaceae plants, namely Codonopsis Codonopsis Codonopsis pliosula (Franch) Nannf, Suhua Codonopsis Codoncpsis pilosula Nannf.var.modesta (Nannf) L.T.Shen or Sichuan Codonopsis Codonopisis tangshen Dried root of Oliv. [1] . Codonopsis pilosula has the functions of invigorating the middle and replenishing qi, promoting body fluid and harmonizing the stomach, invigorating the spleen and benefiting the lungs, etc. It is a traditional tonic medicine in my country and can be used as a substitute for ginseng [2-4] . The main pharmacological effects of Atractylolide, an index component in Codonopsis Codonopsis...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/92
CPCC07D307/92
Inventor 樊秦夏鹏飞彭雪晶赵磊张艳霞
Owner GANSU UNIV OF CHINESE MEDICINE
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