Method for determining content of nineteen components in radix stephaniae tetrandrae and astragalus membranaceus soup by ultra-high performance liquid chromatography tandem mass spectrometry

A technology of ultra-high performance liquid phase and Fangji Huangqi Decoction, which is applied in the direction of measuring devices, material separation, and analysis of materials, can solve problems such as difficult to truly control the quality of drugs, and achieve good reproducibility, good separation, and short analysis time. Effect

Pending Publication Date: 2020-06-12
SHANXI UNIV
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Problems solved by technology

In traditional Chinese medicine, it is difficult to control the quality of a single active ingredient or index ingredient, and the method of conten...

Method used

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  • Method for determining content of nineteen components in radix stephaniae tetrandrae and astragalus membranaceus soup by ultra-high performance liquid chromatography tandem mass spectrometry
  • Method for determining content of nineteen components in radix stephaniae tetrandrae and astragalus membranaceus soup by ultra-high performance liquid chromatography tandem mass spectrometry
  • Method for determining content of nineteen components in radix stephaniae tetrandrae and astragalus membranaceus soup by ultra-high performance liquid chromatography tandem mass spectrometry

Examples

Experimental program
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Effect test

preparation example Construction

[0021] (1) Preparation of the test solution: Accurately weigh 35 mg and 300 mg of Fangji Huangqi Tang freeze-dried powder into a centrifuge tube, add 1 mL of methanol, vortex for 1 min to mix, and perform ultrasonic treatment for 30 min (temperature: 30 ° C, Frequency: 30KHz), centrifuged at 13000r / min for 15min, and the supernatant was taken to obtain the test solution No. 1 and No. 2, which were used for ultra-high performance liquid chromatography tandem mass spectrometry positive and negative ion mode analysis respectively;

[0022] (2) Preparation of the reference substance solution: take formononetin, formononetin, calycosin, acteosin, pterostalane, pteroside, isoflavane, liquiritigenin, liquiritin, glycyrrhetinic acid, and tetrandrol Accurately weigh the reference substances of alkali, fangcinoline, atractylodes lactone Ⅰ, atractylodes lactone Ⅱ Ⅰ, isoflavane, astragaloside Ⅰ, astragaloside Ⅱ, astragaloside Ⅲ and astragaloside Ⅳ, and place them in 5 mL volumetric flasks ...

example 2

[0030] Example 2: Methodological investigation of the content determination of nineteen components in Fangji Huangqi Decoction: the test solutions for the following experiments were all prepared by the following method: Take Fangji Huangqi Decoction powder, weigh 35 mg and 300 mg accurately, add 1 mL of methanol, and extract by ultrasonic 30min (temperature: 30°C, frequency: 30KHz), centrifuge at 13000r / min for 15min, take the supernatant, and filter it with a 0.22μm microporous membrane to obtain the test solution, which is used for mass spectrometry positive and negative ion mode analysis respectively.

[0031] Establishment of the standard curve and linear range test: Dilute the mixed standard solution A to a final concentration of 100%, 75%, 50%, 30%, 10%, and 2%, and dilute the mixed standard solution B to the final concentration. The concentration is 60%, 40%, 20%, 7%, 5%, 2% series concentration. Using the proposed method, Waters ACQUITY UPLC HSS T3 (2.1mm×100mm, 1.8μm)...

example 3

[0043] Example 3 Determination of the content of nineteen components in Fangji Huangqi Decoction: use the determination conditions for the content of the nineteen components established above to determine the content of Fangji Huangqi Decoction: accurately weigh 35 mg and 300 mg of the freeze-dried powder of Fangji Huangqi Decoction in a centrifuge tube Add methanol 1mL, vortex for 1min to mix, carry out ultrasonic treatment for 30min (temperature: 30°C, frequency: 30KHz), centrifuge at 13000r / min for 15min, take the supernatant, that is, the test solution No. 1 and No. 2 No.

[0044] Using MRM multiple reaction monitoring mode, ESI ion source, ion source temperature 400 ℃, mass range: M / Z 50-1500, spray voltage: 3.5 kV (+), 3.5 kV (-), sheath gas Volume: 35, auxiliary volume: 10, capillary temperature: 320°C, lens voltage: 55 kPa, mass resolution: 70000;

[0045] The standard curve method was used to calculate the contents of nineteen components in the test product, and the ...

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Abstract

The invention belongs to the technical field of traditional Chinese medicine component detection and provides a method for determining the content of nineteen components in radix stephaniae tetrandraeand astragalus membranaceus soup by ultra-high performance liquid chromatography-tandem mass spectrometry. The method comprises the following steps of pespectively preparing a test solution, a reference solution and a mixed standard solution; detecting the mixed standard substance solution by ultra-high performance liquid chromatography-tandem mass spectrometry, drawing a standard curve and a test solution, performing mass spectrometry positive and negative ion mode analysis by ultra-high performance liquid chromatography-tandem mass spectrometry, and obtaining the contents of nineteen components in the radix stephaniae tetrandrae and astragalus membranaceus soup according to the standard curve. The method is high in sensitivity and good in reproducibility; analysis accuracy and reliability, 19 chemical components in the radix stephaniae tetrandrae and radix astragali soup can be quantitatively detected at the same time; formononetin, formononetin, calycosin-7-one, calycosin-7-one, pterocarpan, pterocarpan, isoflavane, liquiritin, glycyrrhetinic acid, tetrandrine, tetrandrine, atractylodes lactone I, atractylodes lactone II I, isoflavane, astragaloside I, astragaloside II, astragaloside III and astragaloside IV.

Description

technical field [0001] The invention belongs to the technical field of detection of traditional Chinese medicine components, and in particular relates to a method for determining the contents of nineteen components in Fangji Huangqi Decoction by ultra-high performance liquid chromatography tandem mass spectrometry. Background technique [0002] Fangji Huangqi Decoction was first recorded in "Synopsis of the Golden Chamber". The whole prescription is composed of Fangji, Astragalus, Atractylodes macrocephala, licorice, ginger, and jujube. In recent years, the clinical application of Fangji Huangqi Decoction mainly focuses on chronic heart failure, cardiogenic edema, rheumatoid arthritis, chronic glomerulonephritis, nephrotic syndrome and other diseases. to receive more and more attention. However, most of the existing studies focus on the clinical and pharmacological effects, and less research on its chemical constituents. In order to better study Fangji Huangqi Decoction, e...

Claims

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Application Information

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IPC IPC(8): G01N30/88G01N30/06G01N30/34G01N30/72
CPCG01N30/88G01N30/06G01N30/34G01N30/72G01N2030/884
Inventor 李爱平杨柳秦雪梅张丽增
Owner SHANXI UNIV
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