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Method for determining content of chemical components in chrysanthemum

A technology of chemical composition and content, applied in the field of determination of chemical composition content in chrysanthemum, can solve the problems of imperfect quality control system and large quality difference of chrysanthemum medicinal materials, and achieve the effect of high sensitivity, strong specificity and fast analysis speed

Active Publication Date: 2020-08-14
TIANJIN UNIV OF TRADITIONAL CHINESE MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are various kinds of chrysanthemum medicinal materials on the market and different origins, resulting in large differences in the quality of chrysanthemum medicinal materials, and its quality control system is not perfect

Method used

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  • Method for determining content of chemical components in chrysanthemum
  • Method for determining content of chemical components in chrysanthemum
  • Method for determining content of chemical components in chrysanthemum

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] 1. Determine the chromatographic conditions

[0042] Chromatographic column: ACQUITY UPLC BEH C18 column (2.1×100mm, 1.7μm); mobile phase: phase A is 0.1% formic acid water, phase B is acetonitrile; gradient elution, elution program: 0-2min, 6%-25 %B; 2-4min, 25%-26%B; 4-7min, 26%-75%B, 7-8min, 75%-95%B. Flow rate: 0.3mL / min; column temperature: 20°C; injection volume: 5μL.

[0043] 2. Determination of mass spectrometry conditions

[0044] Electrospray ion source (ESI) is used, with multiple reaction ion monitoring (MRM) as the detection mode, negative ion full scan mode; capillary voltage: 4000V; capillary temperature is set to 300°C, dry gas flow rate is 7L / min; atomizer pressure is 35psi . The ion pairs and mass spectrometry parameters of the 13 analytes are shown in Table 1.

[0045] Table 1 Ion pairs and mass spectrometry parameters information of 13 compounds in chrysanthemum

[0046]

[0047] 3. Preparation of mixed reference substance stock solution

[...

Embodiment 2

[0054] Embodiment 2 establishes standard curve

[0055] Accurately measure an appropriate amount of the mixed reference substance stock solution prepared in Example 1, use methanol as a solvent, and carry out gradient dilution of the mixed reference substance stock solution with 2, 2, 2, 2.5, 2, 2.5, 2 times successively to obtain 8 For the mixed reference substance solutions of four concentrations, 8 concentrations of mixed reference substance solutions were taken respectively, and 5 μL of sample injection was analyzed to obtain the multiple reaction ion monitoring spectra of each reference substance at different concentrations, wherein, the mixed control substance after the second dilution The multiple reaction ion monitoring chromatogram of the sample solution is as follows figure 1 As shown in figure a. With the concentration of the analyte (X) as the abscissa and the peak area of ​​the analyte (Y) as the ordinate, the weighted least square method is used for regression c...

Embodiment 3

[0058] Embodiment 3 precision test

[0059] 1. Intra-day precision: prepare the mixed reference substance stock solution according to the method of Example 1, inject samples continuously for 6 times according to the chromatographic conditions and mass spectrometry conditions of Example 1, and obtain the peak area of ​​each compound, see Table 4, record 13 kinds of chemical compounds The peak area of ​​the components was used to calculate the RSD value, and the results showed that the intraday precision of this method was good.

[0060] Table 4 Intraday precision experiment data table of 13 components of chrysanthemum (n=6)

[0061]

[0062]

[0063] 2. Day-to-day precision: prepare the mixed reference substance stock solution according to the method in Example 1, repeat the sample injection 2 times according to the chromatographic conditions and mass spectrometry conditions in Example 1, and record the peak areas of 13 chemical components for three consecutive days , to...

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Abstract

The embodiment of the invention provides a method for determining the content of chemical components in chrysanthemum, which adopts ultra-high performance liquid chromatography-mass spectrometry to determine the content of 13 chemical components in chrysanthemum at the same time. The 13 chemical components comprise isochlorogenic acid C, hesperidin, coreopsis tinctoria glycoside, quercetin, farnetin, hyperoside, chlorogenic acid, luteolin-7-O-glucuronide, unuronide, luteolin, apigenin, diosmetin, isoquercitrin and cryptochlorogenic acid. By adopting the method disclosed by the invention, the contents of 13 chemical components in the chrysanthemum can be simultaneously determined by reasonably selecting chromatographic conditions and mass spectrometric conditions. And the method has the advantages of simplicity, convenience, high sensitivity, high analysis speed, strong specificity and the like, so that the method can be used for controlling the quality of the chrysanthemum medicinal material.

Description

technical field [0001] The invention relates to the technical field of determination of components of traditional Chinese medicines, in particular to a method for determining the content of chemical components in chrysanthemums. Background technique [0002] Chrysanthemum, the name of traditional Chinese medicine, is the dry flower head of Chrysanthemum morifolium Ramat. in the family Compositae. Indications for wind-heat and cold, febrile disease at the onset, liver-yang dizziness, liver-wind excess syndrome, conjunctival congestion, blurred vision, sore carbuncle and swollen toxin. Chrysanthemum contains flavonoids, volatile oils, organic acids, sugars and amino acids and other chemical components, flavonoids and organic acids are its main active ingredients. At present, there are various types of chrysanthemum medicinal materials in the market and different origins, resulting in large differences in the quality of chrysanthemum medicinal materials, and its quality contro...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/72G01N30/86
CPCG01N30/02G01N30/06G01N30/7266G01N30/8682G01N2030/065
Inventor 何俊贾琪欧阳慧子王维常艳旭
Owner TIANJIN UNIV OF TRADITIONAL CHINESE MEDICINE
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