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
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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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