Method for online determination of furocoumarin content based on combination of MSPD extraction and FESI-MCDS-MEKC

A furanocoumarin and content technology, which is applied in the field of analysis and detection, can solve problems such as the need to improve the sensitivity, and achieve the effects of improving the detection sensitivity, orderly pore size distribution, and short analysis time.

Active Publication Date: 2021-02-26
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] However, the enrichment multiples of these methods are mostly only a few times - dozens of times, and their sensitivity still needs to be improved

Method used

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  • Method for online determination of furocoumarin content based on combination of MSPD extraction and FESI-MCDS-MEKC
  • Method for online determination of furocoumarin content based on combination of MSPD extraction and FESI-MCDS-MEKC
  • Method for online determination of furocoumarin content based on combination of MSPD extraction and FESI-MCDS-MEKC

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Mix 25 mg of Angelica dahurica powder with 50 mg of molecular sieve KIT-6, and grind for 150 seconds to obtain a mixed powder. The mixed powder is eluted with a solid-phase extraction column, and the eluent is 500 μL of methanol. After the elution is completed, the obtained eluent is placed in Extracts were obtained by evaporating methanol to dryness in a fast solvent evaporator.

[0056] Pre-treat the capillary. Before use, the new capillary column needs to be treated with NaOH (1mol / L, 20min), NaOH (0.1mol / L, 10min), pure water (10min) and buffer solution (5min) at a pressure of 50mbar before use. rinse activation;

[0057] The extract was redissolved with 20mmol / L sodium lauryl sulfate to obtain an extract solution in which the sample matrix was sodium lauryl sulfate.

[0058] Carry out electrophoresis analysis based on FESI-MCDS-MEKC again and obtain the peak area of ​​furanocoumarin in the extract (extract), the peak area is substituted into corresponding standard...

Embodiment 2

[0062] Embodiment 2, MSPD condition optimization

[0063] (1) Influence of the type of adsorbent

[0064] Referring to the method of Example 1, using Angelica dahurica as an actual sample, the influence of molecular sieves on the enrichment effect of MSPD was investigated.

[0065] The effects of two kinds of molecular sieves KIT-6 and SPA-16 and other traditional adsorbents florisil, alumina and silica gel on the extraction efficiency of MSPD were investigated. The results are as follows: image 3 shown. The results showed that the extraction of the two target analytes was the best when KIT-6 was used as the adsorbent. This may be because its 3D three-dimensional structure increases the specific surface area, and the sample can be more fully in contact with the adsorbent. Therefore, KIT-6 was chosen as the adsorbent.

[0066] (2) The effect of the ratio of sample to adsorbent

[0067] Referring to the method of Example 1, using Angelica dahurica as an actual sample, the ...

Embodiment 3

[0078] Embodiment 3, FESI-MCDS-MEKC condition optimization

[0079] (1) The influence of the organic solvent in the buffer

[0080] Referring to the method of Example 1, the concentration of the standard substance was 1 μg / mL, and Angelica dahurica was used as the actual sample to investigate the influence of the organic solvent in the buffer solution on the enrichment effect of MSPD.

[0081] The organic solvent in the buffer solution (BGE) will affect the magnitude of the electroosmotic flow and thus indirectly affect the separation process. This experiment investigated the peak situation of three analytes when the methanol content was 0%, 10%, 20% and 30%, the results are as follows Figure 8 shown. It can be seen from the figure that when no methanol was added to the buffer, the peaks of the three analytes could not be separated. When the methanol content was 10% and 20%, the peaks of notopteryl alcohol and isoimperatorin were not completely separated. Only when the me...

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Abstract

The invention discloses a method for the online determination of furocoumarin content based on combination of MSPD extraction and FESI-MCDS-MEKC, which comprises the following steps: mixing a sample to be detected with an adsorbent, pulverizing to obtain mixed powder, eluting the mixed powder with a solid phase extraction column, collecting effluent, and volatilizing a solvent to obtain an extract; respectively pretreating a capillary tube and the extract, carrying out electrophoretic analysis on the basis of the FESI-MCDS-MEKC to obtain the peak area of furocoumarin in the extract, and substituting the peak area into a corresponding standard curve to obtain the content of furocoumarin in the sample to be detected. The method is simple and convenient to operate, short in analysis time, high in separation efficiency, accurate, reliable and good in reproducibility, the enrichment multiple reaches 302 times, and the contents of notopterol, isoimperatorin and imperatorin in the sample to be detected can be accurately determined.

Description

technical field [0001] The invention relates to the technical field of analysis and detection, in particular to a method for online determination of furanocoumarin content based on MSPD extraction combined with FESI-MCDS-MEKC. Background technique [0002] Furanocoumarins are a class of lactone compounds containing benzoα-pyrone structure that exist in plants, animals and microbial metabolites. They have various biological activities such as analgesic and anti-inflammatory, antimicrobial, anticonvulsant and anticancer , are also widely used in the pharmaceutical industry, but their phototoxicity has also attracted widespread attention from scholars. [0003] Under the irradiation of ultraviolet light, a small amount of furanocoumarins may cause skin burns, even without ultraviolet light irradiation, high doses of furanocoumarins showed toxicity to different tissues of mice. Therefore, furanocoumarins are listed as prohibited substances in China's cosmetics industry regulati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/08G01N30/86G01N27/447
CPCG01N30/02G01N30/06G01N30/08G01N30/8675G01N27/447G01N2030/062
Inventor 楚楚刘彩婧连琳敏杨斐童胜强颜继忠
Owner ZHEJIANG UNIV OF TECH
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