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Derivation-based detection analysis method for ginsenoside and aglycone thereof

A technology of ginsenoside aglycon and ginsenoside, which is applied in the field of analytical chemistry and can solve problems such as long reaction time

Inactive Publication Date: 2015-01-28
QUFU NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The purpose of the present invention is to provide a detection and analysis method based on derivatized ginsenosides and their aglycones. For the first time, 4'-carboxyrhodamine is used to derivatize the active hydroxyl groups in ginsenosides and their aglycones, and acetonitrile is used to replace The traditional highly volatile and irritating pyridine is used as a solvent, and the problem of long reaction time is solved.

Method used

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  • Derivation-based detection analysis method for ginsenoside and aglycone thereof
  • Derivation-based detection analysis method for ginsenoside and aglycone thereof
  • Derivation-based detection analysis method for ginsenoside and aglycone thereof

Examples

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Effect test

Embodiment 1

[0042] Detection of Ginsenoside Aglycone PD and PT in Ginseng Medicinal Materials

[0043] 1. Ultrasonic-Assisted-Dispersion Liquid-Liquid Microextraction of Ginsenoside Aglycone PD and PT

[0044] Weigh 1.0 g of ginseng medicinal powder (purchased from Tongrentang pharmacies in Beijing, Changchun, and Jinan), and carry out extraction treatment and acid hydrolysis according to the literature method, so that the ginsenosides in the medicinal materials can be converted into PD and PT (Physical and Chemical Test-Chemical Volume, 2010, 46 (5): 482-484) for micro-extraction: draw 5ml of the above sample solution into a conical centrifuge tube, add 500 μL of ethanol as a dispersant, 150 μL of chloroform as an extraction agent, and then add 4.35 mL of pure water to make the total volume 10 mL, ultrasonically assisted-dispersion liquid-liquid microextraction at room temperature for 3 min, centrifuged for 2 min (12000 rpm), absorb the lower organic phase and blow it to dryness with nit...

Embodiment 2

[0059] Detection of Ginsenosides and Its Aglycones in Rat Plasma

[0060] 1. Ultrasonic-assisted dispersion-liquid-liquid microextraction of ginsenosides and their aglycones

[0061] Take 50 μL of deproteinized rat plasma containing ginsenosides and its aglycones into a centrifuge tube, dilute to 2 mL (pH 5-7) with deionized water, and quickly inject 80 μL of chloroform and 300 μL mixed solution of methanol. After ultrasonic treatment for 2 min, a uniform emulsion system was formed. Put the solution into a high-speed centrifuge and centrifuge for 3 min at a speed of 10000 r / m. After centrifugation, the organic phase was deposited at the bottom of the centrifuge tube. Use a micro-syringe to absorb the deposited phase and transfer it to another vial. After blowing dry with nitrogen gas, redissolve it in an appropriate amount of acetonitrile to obtain a concentration of 2.0 × 10 -5 mol / L extracts of ginsenosides and their aglycones.

[0062] 2. Derivatization reaction of gin...

Embodiment 3

[0067] Detection of Ginsenosides and Its Aglycones in Rat Plasma

[0068] 1. Ultrasonic-assisted dispersion-liquid-liquid microextraction of ginsenosides and their aglycones

[0069] Take 50 μL of deproteinized rat plasma containing ginsenosides and its aglycones into a centrifuge tube, and dilute to 2 with deionized water.

[0070]mL (pH value 5-7), quickly inject a mixed solution containing 100 μL chloroform and 350 μL methanol. After ultrasonic treatment for 2 min, a uniform emulsion system was formed. Put the solution into a high-speed centrifuge and centrifuge for 3 min at a speed of 10000 r / m. After centrifugation, the organic phase was deposited at the bottom of the centrifuge tube. Use a micro-syringe to absorb the deposited phase and transfer it to another vial. After blowing dry with nitrogen gas, redissolve it in an appropriate amount of acetonitrile to obtain a concentration of 2.0 × 10 -5 mol / L extracts of ginsenosides and their aglycones.

[0071] 2. Derivat...

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Abstract

The invention relates to a derivation-based detection analysis method for ginsenoside and aglycone thereof. According to the method, a derivatization reagent 4'-carboxyrhodamine is used for derivatizing free hydroxyl in ginsenosides and aglycones thereof, and a mass spectrum sensitization analysis method employing ultra-high performance liquid chromatography triple-quadrupole mass spectrum detection analysis with multiple reaction monitoring modes is utilized. The method is applicable to analyze and detect 10 ginsenosides and 4 ginsenoside aglycones, by calculating and analyzing a detection result, the content of ginsenosides and aglycones can be accurately obtained. The method is high in sensitivity, excellent in accuracy and good in selectivity, is capable of substantially improving the matrix effect, and has important meaning on pharmacology, medicament screening, ginseng medicinal material and ginseng related product quality control.

Description

technical field [0001] The invention relates to the field of analytical chemistry, in particular to a detection and analysis method based on derivatized ginsenosides and their aglycones, in particular to a method for derivatizing the active hydroxyl groups of ginsenosides and their aglycones by using 4'-carboxyrhodamine A mass spectrometry-enhanced analysis method for detection and analysis by ultra-high performance liquid chromatography triple quadrupole mass spectrometry. Background technique [0002] Ginsenoside is the main active ingredient in ginseng. Many studies have reported that ginsenoside has anti-cancer and health care effects. The vast majority of ginsenosides can be divided into protopanaxadiol (PPD) and protopanaxatriol (PPT) types according to their aglycon structures, and protopanaxadiol (PPD) and protopanaxatriol (PPT) are also It is considered to be the final metabolite of ginsenosides in vivo and reflects its pharmacological activity. Ginsenosides have ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/08
Inventor 赵先恩朱树芸尤进茂吕涛
Owner QUFU NORMAL UNIV