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Anthraquinone derivative bonded silica gel stationary phase used for ginsenoside detection as well as preparation method thereof

An anthraquinone derivative-bonded silica gel technology is applied in the field of analysis and detection, and can solve the problems of poor stability of the mobile phase, cumbersome preparation of the chiral mobile phase, and must be prepared immediately for immediate use. The effect of the separation effect

Inactive Publication Date: 2018-12-21
林思思
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent CN107505409A discloses a method for separating ginsenoside RZ1 and ginsenoside RK1, which uses a chiral mobile phase addition method based on reversed-phase silica gel column chromatography. Although the separation is good, the chiral mobile phase preparation It is cumbersome and must be prepared immediately before use, and the stability of the mobile phase is poor

Method used

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  • Anthraquinone derivative bonded silica gel stationary phase used for ginsenoside detection as well as preparation method thereof
  • Anthraquinone derivative bonded silica gel stationary phase used for ginsenoside detection as well as preparation method thereof
  • Anthraquinone derivative bonded silica gel stationary phase used for ginsenoside detection as well as preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] Example 1: Preparation and packing of anthraquinone derivative bonded silica gel stationary phase

[0065] 1. The chemical structural formulas of anthraquinone derivatives A to D are as follows: figure 1 As shown, they are 1,2-dihydroxyanthraquinone, 2,6-dihydroxyanthraquinone, 1,4-dihydroxyanthraquinone, and 1,8-dihydroxyanthraquinone.

[0066] Two, the preparation steps of anthraquinone derivatives A~D bonded silica gel stationary phase are as follows:

[0067] Step S1, first soak the silica gel (spherical silica gel, particle diameter 5 μm, pore diameter with 3mol / L hydrochloric acid The specific surface area is 450m 2 / g, purchased from Saifen Technology) for 12 hours, reheated and refluxed for 10 hours, then repeatedly washed with water until neutral, and finally washed twice with acetone, baked at 160°C for dehydration and activated for 6 hours, cooled and stored in a desiccator for later use ;

[0068] Step S2, take 6.0g of activated dry silica gel, add 80mL...

Embodiment 2

[0072] Example 2: The separation effect of anthraquinone derivative A bonded to silica gel relative to ginsenoside RZ1 and RK1

[0073] The purity of ginsenoside RZ1 and ginsenoside RK1 reference substance is not less than 98%.

[0074] Preparation of mixed reference substance solution: Accurately weigh 10 mg each of ginsenoside RZ1 and ginsenoside RK1 reference substance, put them in a 20ml measuring bottle, dissolve with acetonitrile and constant volume, shake well to obtain a mixed reference substance solution.

[0075] HPLC chromatographic parameters:

[0076] Chromatograph: Waters2695 high performance liquid chromatograph;

[0077] Chromatographic column: anthraquinone derivative A bonded silica gel chromatographic column (150×4.6mm, see Example 1 for the preparation method);

[0078] Mobile phase A phase: water;

[0079] Mobile phase B phase: acetonitrile;

[0080] Elution program: 0-5min, 35%B; 5-20min, 35%→85%B;

[0081] Flow rate: 1.0mL / min;

[0082] Column temp...

Embodiment 3

[0086] Example 3: The separation effect of anthraquinone derivative B bonded to silica gel relative to ginsenoside RZ1 and RK1

[0087] The purity of ginsenoside RZ1 and ginsenoside RK1 reference substance is not less than 98%.

[0088] Preparation of mixed reference substance solution: Accurately weigh 10 mg each of ginsenoside RZ1 and ginsenoside RK1 reference substance respectively, put them in a 20ml measuring bottle, dissolve with acetonitrile and constant volume, shake well to obtain a mixed reference substance solution.

[0089] HPLC chromatographic parameters:

[0090] Chromatograph: Waters2695 high performance liquid chromatograph;

[0091] Chromatographic column: anthraquinone derivative B bonded silica gel chromatographic column (150×4.6mm, see Example 1 for the preparation method);

[0092] Mobile phase A phase: water;

[0093] Mobile phase B phase: acetonitrile;

[0094] Elution program: 0-5min, 35%B; 5-20min, 35%→85%B;

[0095] Flow rate: 1.0mL / min;

[0096...

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Abstract

The invention discloses an anthraquinone derivative bonded silica gel stationary phase used for ginsenoside detection as well as a preparation method thereof. The invention finds that separation effect of silica gel on ginsenosides RZ1 and RK1 can be obviously improved by bonding 1,2-dihydroxy anthraquinone, 2,6-dihydroxy anthraquinone or 1,8-dihydroxy anthraquinone on the surface of the silica gel. The 1,2-dihydroxy anthraquinone, 2,6-dihydroxy anthraquinone, 1,4-dihydroxy anthraquinone and 1,8-dihydroxy anthraquinone are of a dihydroxy anthraquinone structure respectively, but bonding of the1,4-dihydroxy anthraquinone can not enhance separating power of the silica gel on the ginsenosides RZ1 and RK1, and the phenomenon can be related to positions of hydroxyls. Therefore, a chromatographic column with 1,2-dihydroxy anthraquinone, 2,6-dihydroxy anthraquinone or 1,8-dihydroxy anthraquinone bonded silica gel filler can be produced and prepared to be taken as an analysis chromatographiccolumn specially used for the ginsenosides RZ1 and RK1, cost is low, and an application method is simple.

Description

technical field [0001] The invention belongs to the field of analysis and detection, and relates to the separation of isomer compounds, in particular to an anthraquinone derivative-bonded silica gel stationary phase for ginsenoside detection and a preparation method thereof. Background technique [0002] Ginsenosides are the main active ingredients of Panax genus plants such as the famous and precious medicinal materials Panax ginseng and American ginseng, which have good pharmacological activities such as anti-tumor, anti-inflammatory, anti-oxidation and inhibition of cell apoptosis. [0003] There are many kinds of ginsenosides, among which there are many pairs or groups of isomers. Some isomers have very similar chemical polarity, which makes the separation and analysis of these isomers more difficult. Taking ginsenosides RZ1, RK1 and RG5 as an example, the three are isomers of each other. From the biogenic pathway, the C20 hydroxyl of ginsenoside RG3 and the C21 hydroge...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 林思思
Owner 林思思