Method for extracting and purifying flavones and phenolic acids in medicinal material ixeris sonchifolia through metal ion chelation
A technology of metal ions and bitter dishes, which is applied in the field of medicine, can solve the problems of many steps, complicated process, and long extraction cycle, and achieve the effects of good fluidity, simplified extraction process steps, and shortened extraction cycle
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Embodiment 1
[0017] Example 1: Detection of luteolin-7-O-β-D-glucuronide (LGU) and cichoric acid (CCA) in samples by HPLC-UV method.
[0018] High-performance liquid chromatography is used for detection, and the chromatographic equipment and chromatographic conditions are as follows: SHIMADZULC-2010A (autosampler, column thermostat, quaternary pump, UV detector, Class-VP operating system); chromatographic column: Ultimate? AQC- 18 columns (250mm×4.6mm, 5μm, Welch Materials Inc.); mobile phase: A: methanol-tetrahydrofuran (volume ratio = 15:1); B: water (1% formic acid), using a gradient elution program, 0-45min: 30%A; 45-52min: 80%A; 52-60min: 30%A; the flow rate is 1mL / min, the column temperature is 40°C, the detection wavelength is 348nm, and the injection volume is 10μL.
[0019] Calculate the establishment of the standard curve.
[0020] Accurately weigh an appropriate amount of LGU and CCA standard substances after vacuum drying, dissolve them with chromatographic methanol to obtain ...
Embodiment 2
[0027] Different metal ions Mg 2+ , Ca 2+ , Zn 2+ Purification process and results of flavonoids (represented by LGU) and phenolic acids (represented by CCA).
[0028] 1 kg of Kudiezi medicinal material was reflux extracted with 15 and 12 times the amount of 50% ethanol for 2 times, each time for 1 hour. The extracts are combined, the ethanol is recovered under reduced pressure until there is no alcohol smell, the obtained suspension is dried by spray drying, and the obtained product is collected and protected from moisture for later use. Accurately weigh an appropriate amount of dried Kudiezi extract, use methanol to prepare a solution with a concentration of 1mg / mL through ultrasonic oscillation, and filter for later use. Take Kudiezi filtrate 100ml, add 0.1mol / L metal salt (MgCl 2 , CaCl 2 , ZnCl 2 ) of methanol solution, and after fully shaking for 15 minutes, add dropwise 1mol / L NaOH solution to adjust the pH value of the solution. Stand for 4 hours, filter, and wa...
Embodiment 3
[0031] Fourier Transform Infrared Spectroscopy (FT-IR).
[0032] Weigh an appropriate amount of vacuum-dried samples, mix them with dry KBr, and press them into tablets. Use an infrared spectrometer (IFS-55, Bruker, Germany) to measure the Fourier infrared spectrum, scanning range: 4000-400cm -1 .
[0033] The infrared spectrum of Kudiezi ethanol 50% extract, Kudiezi extract magnesium ion precipitate (pH9) is as follows Figure 4 , 5 shown. There is a hydroxyl vibration peak formed around 3427. 1628-1629, 1384cm -1 Nearby are the asymmetric and symmetric stretching vibration peaks of the carbonyl group, 1264 and 1068cm -1 are the asymmetric and symmetric stretching vibration absorption peaks of the C-O-C group. 1115-1121cm -1 is the C-O absorption peak. The absorption peak range of MgO is 500-1000cm -1 , peak at 860cm -1 . Figure 5 Medium 1500cm -1 The enhancement of the nearby vibration peaks indicates that the content of aromatic ring substances has increased, t...
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