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Method for extracting xanthinosin from xanthium sibiricum

A technology of cocklebur saponin and cocklebur, applied in the direction of organic chemistry, which can solve the problems of large difference in cocklebur saponin content, low cocklebur saponin content, cumbersome extraction technology, etc., to achieve industrial application and low cost , the effect of high purity

Pending Publication Date: 2019-09-27
GUANGXI BOTANICAL GARDEN OF MEDICINAL PLANTS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The chemical structural formula of cocklebur saponin is: Among the sesquiterpene lactone compounds, the content of cocklebur saponin with the highest pharmacological activity is low, and the content of cocklebur saponin in different samples is quite different and uneven. In terms of the separation and extraction of cocklebur chemical components, there are currently The extraction technology is cumbersome, the efficiency is low and the purity is not high, etc.

Method used

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  • Method for extracting xanthinosin from xanthium sibiricum
  • Method for extracting xanthinosin from xanthium sibiricum

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042]Take 5 grams of cocklebur powder, add 10 ml of cellulase for extraction, add 30 ml of buffer solution (NaAc-HAc buffer solution with a pH of 4.5), heat in a water bath at 45 degrees, and inactivate at high temperature for 5 minutes after 2 hours, add 100 ml of bionic Extract (0.9% sodium chloride, 0.32% pepsin, 0.02mol / L hydrochloric acid), ultrasonic 40min, filter after cooling, take 20ml of filtrate, evaporate to dryness in water bath, add methanol to dissolve and transfer to volumetric flask to constant volume, filter, enter High-performance liquid chromatography detection, wherein, chromatographic conditions: chromatographic column: C18 column (column diameter 4.6 mm × length 250 mm, particle size 5 μm); mobile phase acetonitrile-water (35:65), flow rate 1.0mL / min; detection Wavelength: 205nm; Column temperature: 25°C; Xanthin standard reference substance injection volume 10 μL, Xanthium sample injection volume 15 μL, cocklebur saponin standard reference substance is ...

Embodiment 2

[0045] Take 3 grams of cocklebur powder, add 10 ml of cellulase to extract, add 30 ml of buffer solution (NaAc-HAc buffer solution with a pH of 4.5), heat in a water bath at 45 degrees for 1.5 hours, then inactivate at high temperature for 5 minutes, add 70 ml of bionic extract solution (0.9% sodium chloride, 0.32% pepsin, 0.02mol / L hydrochloric acid), ultrasonic for 30min, filtered after cooling, took 20ml of filtrate, evaporated to dryness in water bath, dissolved in methanol and transferred to a volumetric flask to constant volume, filtered, and entered high-efficiency Detection by liquid chromatography. Among them, chromatographic conditions: chromatographic column: C18 column (column diameter 4.6 mm × length 250 mm, particle size 5 μm); mobile phase acetonitrile-water (35:65), flow rate 1.0mL / min; detection wavelength: 205nm; column temperature: 25°C; the injection volume of the cocklebur saponin standard reference substance is 10 μL, the injection volume of the cocklebur...

Embodiment 3

[0048] Take 6 grams of cocklebur powder and add 10 ml of cellulase for extraction, add 30 ml of buffer solution (NaAc-HAc buffer solution with a pH of 4.5), heat in a water bath at 45 degrees, inactivate at high temperature for 10 minutes after 2.5 hours, add 120 ml of bionic Extract (0.9% sodium chloride, 0.32% pepsin, 0.02mol / L hydrochloric acid), sonicate for 30min, sonicate twice, filter after cooling, take 20ml of filtrate, evaporate to dryness in water bath, add methanol to dissolve and transfer to volumetric flask to constant volume , filter, and enter the high-performance liquid chromatography for detection. Among them, chromatographic conditions: chromatographic column: C18 column (column diameter 4.6 mm × length 250 mm, particle size 5 μm); mobile phase acetonitrile-water (35:65), flow rate 1.0mL / min; detection wavelength: 205nm; column temperature: 25°C; the injection volume of the cocklebur saponin standard reference substance is 10 μL, the injection volume of the ...

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Abstract

The invention provides a method for extracting xanthinosin from xanthium sibiricum. The method comprises the following steps: performing liquid chromatography detection on a xanthium sibiricum sample to screen out high-quality xanthium sibiricum, and then extracting and purifying the high-quality xanthium sibiricum to obtain the xanthinosin, wherein the screening standard of the high-quality xanthium sibiricum is as follows: the chromatographic peak with the same retention time as that of a standard reference material of the xanthinosin has a peak area greater than 50%; or in the absence of the standard reference material, the retention time of the liquid chromatography detection is within 17.5-19.5 minutes, and the peak area of the chromatographic peak of the 205 nm ultraviolet terminal absorption is greater than 50% at the same time. The method provided by the invention can efficiently and quickly detect whether the xanthinosin is contained in the xanthium sibiricum sample, and whether the content meets requirements, and the operation is simple. The method performs purposive extraction and separation on the samples meeting the requirements, so that high-purity xanthinosin can be obtained, and the purity can be up to 98% or above. The method is simple and convenient, the use of expensive large instruments is not needed, the cost is low, and the realization of industrial application is facilitated.

Description

technical field [0001] The invention relates to the technical field of cocklebur saponin extraction. More specifically, the present invention relates to a method for extracting cocklebur saponin from cocklebur. Background technique [0002] Xanthium sibiricum (Xanthium sibiricum) is a plant of the genus Xanthium in the family Asteraceae. It is clinically used to treat symptoms such as wind-cold headache, skin eczema, nasal congestion and runny nose. Bei, Zhao Weixing, Research and application of chemical constituents of cocklebur [J]. Chemical Times, 2011.25(7): 47-49). Xanthane sesquiterpenoids contain a variety of sesquiterpenoids, and have a wide range of biological effects including antibacterial, antiviral, and antitumor (Vasas V, HohmannJ. Xanthane sesquiterpenoids: structure, synthesis and biological activity[J].Nat Prod Rep, 2011, 28(4):824) (Favier LS, Maria AOM, Wendel GH, et al. Anti-ulcergenic activity of xanthanolide sesquiterpenes from Xanthium cavanillesiiii...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/93
CPCC07D307/93
Inventor 乔丽娅夏祥华李小勇
Owner GUANGXI BOTANICAL GARDEN OF MEDICINAL PLANTS
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