HPLC (High Performance Liquid Chromatography) method for separating and detecting atractylenolide II and atractylenolide V

A technique of atractylodes lactone and volume percentage, applied in the field of detection, can solve the problems of separation and detection of the two, and achieve the effect of easy transfer and high repeatability

Active Publication Date: 2017-12-22
国科赛赋河北医药技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The physical and chemical properties of the two are similar, and i

Method used

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  • HPLC (High Performance Liquid Chromatography) method for separating and detecting atractylenolide II and atractylenolide V
  • HPLC (High Performance Liquid Chromatography) method for separating and detecting atractylenolide II and atractylenolide V
  • HPLC (High Performance Liquid Chromatography) method for separating and detecting atractylenolide II and atractylenolide V

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 1. Experimental instruments and materials

[0023] ACQUITY ultra-high performance liquid chromatography (Waters Technology Co., Ltd., USA);

[0024] BT224S electronic balance (Beijing Sartorius Instrument System Co., Ltd.);

[0025] Atractylodes Ⅱ and Atractylodes V are self-made, with a purity greater than 98%;

[0026] Water is ultrapure water, acetonitrile and methanol are chromatographically pure, and other reagents are analytically pure.

[0027] 2. Experimental methods and results

[0028] 1. Solution preparation

[0029] Reference substance solution: Weigh Atractylodes lactone II and Atractylodes lactone V respectively to prepare Atractylodes lactone II reference solution and Atractylodes lactone V reference solution with a concentration of 0.1 mg / mL;

[0030] Test solution: weigh Atractylodes II and Atractylodes V to prepare Atractylodes II 0.5mg / mL and Atractylodes V0.5mg / mL test solutions.

[0031] 2. Chromatographic conditions

[0032] Agilent ZORBAX Ex...

Embodiment 2

[0035] 1. Experimental instruments and materials

[0036] ACQUITY ultra-high performance liquid chromatography (Waters Technology Co., Ltd., USA);

[0037] BT224S electronic balance (Beijing Sartorius Instrument System Co., Ltd.);

[0038] Atractylodes Ⅱ and Atractylodes V are self-made, with a purity greater than 98%;

[0039] Water is ultrapure water, acetonitrile and methanol are chromatographically pure, and other reagents are analytically pure.

[0040] 2. Experimental methods and results

[0041] 1. Solution preparation

[0042] Reference substance solution: weigh Atractylodes lactone II and Atractylodes lactone V respectively with mobile phase to prepare Atractylodes lactone II reference substance solution and Atractylodes lactone V reference substance solution with a concentration of 0.1 mg / mL;

[0043] Test solution: weigh Atractylodes II and Atractylodes V with mobile phase to prepare Atractylodes II 0.5 mg / mL and Atractylodes V 0.5 mg / mL test solution.

[0044]...

Embodiment 3

[0048] 1. Experimental instruments and materials

[0049] ACQUITY ultra-high performance liquid chromatography (Waters Technology Co., Ltd., USA);

[0050] BT224S electronic balance (Beijing Sartorius Instrument System Co., Ltd.);

[0051] Atractylodes Ⅱ and Atractylodes V are self-made, with a purity greater than 98%;

[0052] Water is ultrapure water, acetonitrile and methanol are chromatographically pure, and other reagents are analytically pure.

[0053] 2. Experimental methods and results

[0054] 1. Solution preparation

[0055] Reference substance solution: Weigh Atractylodes lactone II and Atractylodes lactone V respectively to prepare Atractylodes lactone II reference solution and Atractylodes lactone V reference solution with a concentration of 0.1 mg / mL;

[0056] Test solution: weigh Atractylodes II and Atractylodes V to prepare Atractylodes II 0.5mg / mL and Atractylodes V0.5mg / mL test solutions.

[0057] 2. Chromatographic conditions

[0058] Agilent ZORBAX Ex...

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Abstract

The invention discloses an HPLC (High Performance Liquid Chromatography) method for separating and detecting atractylenolide II and atractylenolide V. According to the method, taking octadecylsilane chemically bonded silica (Carbon 18) as a stationary phase, a trifluoroacetic acid-containing organic solvent aqueous solution is taken as a flowing liquid, specifically, the organic solvent aqueous solution is acetonitrile aqueous solution of which the acetonitrile volume percentage concentration is 34 to 38 percent and contains trifluoroacetic acid with the volume percentage concentration of 2.5 to 4.5 percent, or the organic solvent aqueous solution is methyl alcohol aqueous solution of which the methyl alcohol volume percentage concentration is 47 to 51 percent and contains the trifluoroacetic acid with the volume percentage concentration of 2 to 4 percent. According to the HPLC method provided by the invention, the atractylenolide II and the atractylenolide V can be separated effectively; the separation degree is greater than 1.5 and is accordance with regulations; the method only requires a common C18 chromatographic column and a common organic solvent; moreover, gradient elution is not required; the repeatability is high; the common C18 chromatographic column and the common organic solvent are easily transferred among different laboratories.

Description

technical field [0001] The invention belongs to the detection field and relates to the separation and detection of atractylodes lactone, in particular to an HPLC method for separating and detecting atractylodes lactone II and atractylodes lactone V. Background technique [0002] Atractylodes lactones are the main active ingredients of Atractylodes macrocephala, and atractylodes lactones with the following structure have been found so far: [0003] [0004] Among them, Atractylodes lactone II and Atractylodes lactone V are isomers, both of which are formed by dehydration of Atractylodes lactone III. The physical and chemical properties of the two are similar, and it is difficult to separate and detect them by conventional methods. Contents of the invention [0005] The purpose of the present invention is to provide an HPLC method for separating and detecting atractyloid II and atractyloid V. [0006] Realize above-mentioned object technical scheme of the present invent...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 王莉孙天娇胡芳
Owner 国科赛赋河北医药技术有限公司
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