Method for measuring flavone glycoside compounds in herba epimedii

A technology for determination of flavonoid glycosides in A. chinensis, which is applied in the field of determination of Epimedium, can solve the problems of weak anti-interference ability, inaccurate quantification, and difficulty in baseline separation, and achieves the effects of good accuracy, high sensitivity, and easy baseline separation.

Active Publication Date: 2011-02-16
CHINA TOBACCO JIANGXI IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the limitations of resolution, column efficiency, and detector sensitivity, ordinary high-performance liquid chromatography instruments are not easy to achieve baseline separation of these six compounds. In addition, their own weak anti-interference ability may easily lead to inaccurate quantification

Method used

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  • Method for measuring flavone glycoside compounds in herba epimedii

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] a. Weigh 0.5g of the Chinese herbal medicine Epimedium sample of 40 mesh sieves in a 100mL stoppered glass conical flask, add 50mL of 50% methanol-water solution (V / V), weigh, at normal temperature, under ultrasonic power Ultrasonic at 350W and ultrasonic frequency of 70KHz for 30min to make up the weight.

[0016] b. Take the supernatant and filter it with a 0.22um organic phase membrane to obtain the sample to be analyzed.

[0017] c. Analyze the obtained sample to be analyzed:

[0018] 1. Chromatographic conditions: Analytical column: Waters Acquity UPLC BEH C 18 (1.7μm, 2.1mm×50mm); mobile phase: phase A is 0.1% formic acid-water solution (V / V), phase B is acetonitrile solution; gradient condition: 0min, A: B (90%: 10%); 10min, A:B (80%:20%); 25min, A:B (70%:30%); 35min, A:B (50%:50%); 35.1min, A:B (0%:100 %); 39.9 min, A:B (0%:100%) 40.0 min, A:B (90%:10%). Flow rate: 0.25mL / min; column temperature 30°C.

[0019] 2. Mass spectrometry conditions: Quantitative a...

Embodiment 2

[0024] a. Take by weighing 0.4g of the Chinese herbal medicine Epimedium sample of 60 mesh sieves in a 100mL stoppered glass conical flask, add 40mL of 60% methanol-water solution (V / V), weigh, under normal temperature, at a rotating speed of 150r / Shake for 30 minutes at 2 min, let stand for 5 minutes, and make up the weight.

[0025] b. Take the supernatant and filter it with a 0.22um organic phase membrane to obtain the sample to be analyzed.

[0026] c. Analyze the obtained sample to be analyzed:

[0027] 1. Chromatographic conditions: Analytical column: Waters Acquity UPLC BEH C 18 (1.7μm, 2.1mm×50mm); mobile phase: phase A is 0.2% formic acid-water solution (V / V), phase B is acetonitrile solution; gradient condition: 0min, A: B (90%: 10%); 10min, A:B (80%:20%); 25min, A:B (70%:30%); 35min, A:B (50%:50%); 35.1min, A:B (0%:100 %); 39.9 min, A:B (0%:100%) 40.0 min, A:B (90%:10%). Flow rate: 0.25mL / min; column temperature 30°C.

[0028] 2. Mass spectrometry conditions: ...

Embodiment 3

[0030] a. Take by weighing 0.5 g of the Chinese herbal medicine Epimedium sample of 80 mesh sieves in a 100 mL glass conical flask with a stopper, add 20 mL of 70% methanol-water solution (V / V), weigh, and soak for 1.5 h at normal temperature, Make up weight.

[0031] b. Take the supernatant and filter it with a 0.22um organic phase membrane to obtain the sample to be analyzed.

[0032] c. Analyze the obtained sample to be analyzed:

[0033] 1. Chromatographic conditions: Analytical column: Waters Acquity UPLC BEH C 18 (1.7μm, 2.1mm×50mm); mobile phase: phase A is 0.3% formic acid-water solution (V / V), phase B is acetonitrile solution; gradient condition: 0min, A: B (90%: 10%); 10min, A:B (80%:20%); 25min, A:B (70%:30%); 35min, A:B (50%:50%); 35.1min, A:B (0%:100 %); 39.9 min, A:B (0%:100%) 40.0 min, A:B (90%:10%). Flow rate: 0.25mL / min; column temperature 30°C.

[0034] 2. Mass spectrometry conditions: Quantitative analysis was carried out in multiple reaction monitoring...

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Abstract

The patent refers to the field of 'pharmaceutical preparations'. The invention discloses a method for measuring flavone glycoside compounds in herba epimedii, which relates to the field of herba epimedii measurement methods. The method comprises the following steps: (1) crushing leaves of herba epimedii, sieving the crushed material, placing the sieved material in a container, adding 50 to 70 percent aqueous solution of ethanol, extracting the flavone glycoside compounds, collecting supernate, filtering and obtaining samples to be analyzed; and (2) analyzing the obtained samples to be analyzed by using high-performance liquid chromatography and tandem mass spectrometry. The method has the advantages that: the flavone glycoside compounds in herba epimedii can be effectively and completely extracted; analysis is performed through the separation by ultra performance liquid chromatography and specific scanning by the tandem mass spectrometry; and thus, quick, accurate and quantitative analysis is realized.

Description

technical field [0001] The invention relates to an assay method for epimedium, in particular to a assay method for flavone glycosides in epimedium. Background technique [0002] The chemical components in Epimedium Herba, a traditional Chinese medicine, are diverse and very complex. Flavonoid glycosides are one of the important chemical components that are widely distributed, and they are also the main active components. They mainly include icariin A, Huodin A, Epimedin B, Epimedin C, Icariin, Arariin A, etc. These compounds have pharmacological activities such as anti-myocardial ischemia, lowering blood pressure, improving microcirculation, and enhancing immunity. research on them is becoming more and more active. At present, the analysis methods of flavonoid glycosides in Epimedium Herba Epimedium mainly include high performance liquid chromatography and liquid chromatography-mass spectrometry. Due to the limitations of resolution, column efficiency, and detector sensiti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61P9/12G01N30/06A61P37/04G01N30/72A61P9/10G01N30/36G01N30/02A61K36/296
Inventor 郭磊索卫国蔡继宝廖堃洪炜
Owner CHINA TOBACCO JIANGXI IND CO LTD
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