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Purifying method for chicoric acid in echinacea purpurea

A purification method and technology of cichoric acid, applied in chemical instruments and methods, organic chemistry, carboxylate preparation and other directions, can solve the problems of complicated operation steps, cannot guarantee that the product has no residual toxic organic chemical reagents, etc., and achieve simple operation steps. Effect

Active Publication Date: 2015-06-10
CHINA PHARM UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The methods disclosed in the above three inventions have complex operation steps, involve the extraction process, and use toxic chemical reagents, so it cannot be guaranteed that the final product will not have toxic organic chemical reagents residues

Method used

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  • Purifying method for chicoric acid in echinacea purpurea
  • Purifying method for chicoric acid in echinacea purpurea
  • Purifying method for chicoric acid in echinacea purpurea

Examples

Experimental program
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Embodiment 1

[0039] The detection of embodiment 1 cichoric acid

[0040] Preparation of Echinacea purpurea sample solution

[0041] Take the powder of Echinacea purpurea extract, dissolve it with a certain amount of deionized water, sonicate for 30 minutes, filter, then adjust the volume to a suitable volume, prepare a suitable concentration, and the initial pH is 4.35, and use it as a sample solution.

[0042] The detection method of cichoric acid

[0043]Waters C 18 (250mm×4.6mm, 5μm) chromatographic column; mobile phase: 0.2% formic acid solution (A)-methanol (B); flow rate: 1.000mL / min; UV detection wavelength: 330nm; running time: 30min; injection volume: 20μL , Column temperature: 30°C. See Table 1 for liquid phase conditions.

[0044] The liquid chromatogram of Echinacea purpurea extract see figure 1 , the content of cichoric acid in the extract is 4%, the content of caffeoyltartaric acid is 1.3%, and the content of chlorogenic acid is 0.08%.

[0045] Table 1 Conditions of HPL...

Embodiment 2

[0050] The screening of embodiment 2 macroporous adsorption resins

[0051] Combined with the physical and chemical properties of macroporous resins, from the aspects of polarity, particle size, specific surface area, average pore size, etc., select 6 types of macroporous resins: AB-8, HPD826, HPD600, HPD100, DM130, D101, various macroporous resins The physical parameters, see Table 2:

[0052] Table 2 Physical parameters of six types of adsorption resins

[0053]

[0054] The newly purchased macroporous adsorption resin is fully soaked and swollen with 95% ethanol, then washed with distilled water until the effluent is clear, and then set aside.

[0055] Resin regeneration adopts the following method: soak in 5% hydrochloric acid solution for 10 hours, wash with water until neutral; then soak in equal volume of 5% sodium hydroxide solution for 10 hours, wash with water until neutral; finally use 95% ethanol Soak for 10 hours, then wash with water until there is no alcoho...

Embodiment 3

[0068] Example 3 The investigation of the pH value of the sample solution on the adsorption capacity of the macroporous resin

[0069] The pH of the sample solution is a very important factor affecting the adsorption of the macroporous adsorption resin. The pH can affect whether the cichoric acid is in the ion state or the molecular state, thereby changing its polarity, and then affecting the adsorption capacity of the resin. This experiment investigates the effect of pH on the adsorption capacity of HPD100 macroporous adsorption resin, and screens out the optimal pH.

[0070] The configuration of the sample solution is the same as in Example 2: get the powder of the Echinacea purpurea extract, dissolve it with a certain amount of deionized water, ultrasonically 30min, and filter to obtain the subsequent filtrate, which is constant volume in a volumetric flask, and the concentration of cichoric acid is 1.3 mg / mL sample solution, the measured pH is 4.35, with 1mol / L hydrochlori...

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Abstract

The invention discloses a purifying method for chicoric acid in echinacea purpurea. The method comprises the following steps that 1, an echinacea extract is gotten and used for preparing a sample solution with the chicoric acid content being 1.3-5 mg / mL, the pH value of the sample solution is adjusted to 2-5, and then the sample solution serves as a sample loading solution; 2, packing is conducted through a macroporous resin wet method, and the sample loading solution is used for sample loading, wherein the sample loading speed ranges from 2 Bv / h to 3 Bv / h, and the adsorption time ranges from 3 hours to 5 hours; 3, eluting is conducted through deionized water of 0.5-2 Bv, and then ethyl alcohol of 10%-30% is used as an eluting solvent for eluting, wherein the eluting speed ranges from 1 Bv / h to 3 Bv / h; ethyl alcohol eluent of 0.25 Bv to 2.25 Bv is collected and volatilized, and then a chicoric acid product is obtained. By means of the purifying method, the operating steps are simple, no poisonous chemical reagent is used, the purity of the chicoric acid is increased to 85% from 4% through one-time treatment, the number of the purification folds is 21 or more, and the recovery rate is 77% or so.

Description

technical field [0001] The invention belongs to the field of natural medicines, and in particular relates to a method for purifying cichoric acid in Echinacea purpurea. The method avoids the use of a large amount of toxic organic solvents, and has simple steps, high efficiency, safety, environmental protection and low cost. Background technique [0002] Echinacea (Echinacea purpurea) is a perennial herbaceous wild flower of the genus Echinacea in the family Compositae (Compositea) native to America. There are 8 species and several varieties of plants in this genus. The three types that have been developed as medicines are Echinacea purpurea (L.) Moench, E. angustifolia DC. and E. pallida (Nutt) Nutt. Among them, Echinacea (E.purpurea) is an immunostimulant and immunomodulator that is widely valued in the world. Its extract and preparation sales rank among the top 5 in the US pharmaceutical market, and it has received great attention at home and abroad. The chemical composit...

Claims

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Application Information

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IPC IPC(8): C07C69/732C07C67/56
CPCC07C67/56C07C69/732
Inventor 冯锋马健王磊柳文媛曲玮
Owner CHINA PHARM UNIV
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