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A method for enrichment and detection of low-concentration anthraquinone active ingredients

A technology of active ingredients and anthraquinones, applied in the field of natural medicine extraction and detection, can solve the problems of small cross-sectional area, reduced gap, poor repeatability, etc., and achieve the effect of ensuring the degree of adsorption, good reproducibility, and high adsorption effect.

Active Publication Date: 2016-01-20
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Of course, columnar solid phase extraction also has its limitations: small cross-sectional area, low flow rate, easy to block, easy to generate gaps to reduce extraction efficiency, poor repeatability, etc.
This method has not been reported in the extraction and enrichment of traditional Chinese medicine or its biological samples, and it is even blank in the research field of Chinese medicine rhubarb.

Method used

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  • A method for enrichment and detection of low-concentration anthraquinone active ingredients
  • A method for enrichment and detection of low-concentration anthraquinone active ingredients
  • A method for enrichment and detection of low-concentration anthraquinone active ingredients

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] 1 Prepare 200mL of aloe-emodin, rhein, emodin, chrysophanol, and emodin methyl ether with a concentration of 0.25 μg / mL of the reference substance dilution, pH = 6, and add different amounts of rGOFe 3 o 4 Nanoparticles, to obtain mixed solutions with different adsorbent concentrations, the specific preparation method is: take 6 clean 200mL Erlenmeyer flasks with stoppers, numbered 1, 2, 3, 4, 5, 6, add 50 μg / mL reference substance mixed solution 1mL, add 2mg / mL rGOFe on the 1st 3 o 4 40mL of nanoparticle dispersion and 159mL of water with pH=6, add 2mg / mL rGOFe on the 2nd 3 o 4 Nanoparticle dispersion 20mL and pH=6 water 179mL, add 2mg / mL rGOFe on the 3rd 3 o 4 Nanoparticle dispersion 10mL and pH=6 water 189mL, add 2mg / mL rGOFe on the 4th 3 o 4 5mL of nanoparticle dispersion and 194mL of water with pH=6, add 2mg / mL rGOFe on the 5th 3 o 4 Nanoparticle dispersion 2.5mL and pH=196.5mL, add 2mg / mL rGOFe on the 6th 3 o 4 1.25mL of nanoparticle dispersion and 197....

Embodiment 2

[0069] 1 Prepare 200mL of reference substance dilution solution with the concentrations of aloe-emodin, rhein, emodin, chrysophanol and emodin methyl ether at 0.25 μg / mL, pH=6, and add rGOFe 3 o 4 Nanoparticles, so that the concentration of the adsorbent in the mixed solution is 0.05mg / mL, the preparation method is: take 5 clean 200mL Erlenmeyer flasks with stoppers, numbered 1-5, add 194mL of water with pH=6, 50μg / mL reference substance Mixture 1mL, 2mg / mL rGOFe 3 o 4 Nanoparticle dispersion 5mL.

[0070] 2. Put the Erlenmeyer flask containing the mixed solution into the orbital shaker, and shake it for 1 min on No. 1, 2.5 min on No. 2, 5 min on No. 3, 7.5 min on No. 4, and 10 min on No. 5. After standing still, a magnet was placed at the bottom of the Erlenmeyer flask for 5 minutes for adsorption and enrichment.

[0071] 3 After the enrichment is completed, attach the magnet to the bottom of the Erlenmeyer flask, pour and discard the water layer, place the Erlenmeyer fla...

Embodiment 3

[0080] 1 Prepare 200mL of reference substance dilution solution with the concentration of aloe-emodin, rhein, emodin, chrysophanol and emodin methyl ether at 0.25 μg / mL, and add rGOFe 3 o 4 Nanoparticles, so that the concentration of the adsorbent in the mixed solution is 0.05mg / mL, but the pH value is adjusted to 4, 5, 6, 7, 8 respectively. The preparation method is: take 5 clean 200mL conical flasks with stoppers, number 1- 5. 1 mL of 50 μg / mL reference substance mixture, 2 mg / mL rGOFe 3 o 4 Nanoparticle dispersion 5mL, add 194mL of water with pH=4 to No.1, add 194mL of water with pH=5 to No.3, add 194mL of water with pH=6 to No.4, add 194mL of water with pH=7 to No.5, add pH =8 water 194mL.

[0081] 2 Put the Erlenmeyer flask containing the mixed solution into the orbital shaker and shake for 5 minutes. After standing still, a magnet was placed at the bottom of the Erlenmeyer flask for 5 minutes for adsorption and enrichment.

[0082] 3 After the enrichment is complete...

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PUM

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Abstract

The invention provides a method for enrichment and detection of low concentration anthraquinone effective components, the method uses Fe3O4 magnetic graphene (rGO @ Fe3O4) as an adsorbent for extraction and adsorption of a to-be-detected low concentration sample solution, then uses a desorption agent for elution, a solid obtained by drying of the eluant is dissolved, with a dissolution agent to obtain an enrichment sample liquid, the enrichment sample liquid is detected by a liquid chromatograph / mass spectrometer, and the concentration of the anthraquinone effective components in the concentration anthraquinone effective components can be detected by a standard curve and the enrichment factor quantitation. The method can be used for the detection of the low concentration anthraquinone effective components in a rhubarb medicinal material dilution and a biological sample a rat urine sample).

Description

technical field [0001] The invention belongs to the field of natural medicine extraction and detection. It relates to an extraction and detection method of a traditional Chinese medicine and its biological samples, specifically, it involves a magnetic graphene made of ferric iron tetroxide (rGOFe 3 o 4 ) as an adsorbent, a new method for extracting low-concentration traditional Chinese medicine rhubarb rhubarb and its biological samples (rat urine) and detecting the effective components of anthraquinones. Background technique [0002] In the detection of natural product biological samples, sample pretreatment is crucial in the whole experimental process. Through the pretreatment of the sample, the target molecules can be extracted from the complex biological matrix, which can eliminate the interference of the biological matrix on the analysis results. More importantly, in the enrichment process of sample pretreatment, the target molecules can be concentrated through a ser...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/08
Inventor 曹君胡帅帅曹婉庞潇卿
Owner HANGZHOU NORMAL UNIVERSITY
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