A method for separation and detection of flavonoid glycosides in Chinese herbal decoction pieces Fructus Aurantii
A technology of traditional Chinese medicine decoction pieces and flavonoid glycosides, which is applied in the direction of material separation, measuring devices, and analysis materials, and can solve the problems of poor separation effect, poor reproducibility, and low accuracy
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[0039] Preparation of Chitosan Modified Silica Gel Column Stationary Phase
[0040] Soak the silica gel in acid, and reflux, then wash with double distilled water until neutral, wash with acetone three times, bake to remove water and activate, cool and store in a desiccator for later use. Take the activated dry silica gel, add anhydrous dry toluene, and add KH-560 and triethylamine catalyst under stirring. Heated to reflux under the protection of N2, cooled, extracted with toluene, washed with acetone, methanol and acetone in sequence, and dried under vacuum to obtain a coupling agent-bonded silica gel substance, and prepare a silica gel precursor.
[0041] Weigh the silica gel precursor, add chitosan, acetic acid and toluene to it under heating and stirring. Add perchloric acid dropwise as a catalyst, heat to reflux under N2 protection, cool, adjust the pH to neutral, and precipitate solids to obtain the chitosan-modified silica gel column stationary phase.
[0042]As a pre...
Embodiment 1
[0062] (1) Weigh 10 g of Chinese herbal decoction pieces Fructus Aurantii, pulverize with a pulverizer, add 1 L of methanol solvent of analytical grade, and extract by heating to reflux to obtain a crude extract.
[0063] (2) Take 3 g of the crude extract in step (1), add 300 mL of methanol, ultrasonicate, and filter to obtain a filtrate.
[0064] (3) Agilent 1200HPLC high performance liquid chromatography was used to separate the filtrate prepared in step (2).
[0065] The stationary phase is chitosan-modified silica gel; the mobile phase is formic acid solution with a molar concentration of 0.5% and a volume ratio of 70:30 to methanol; the flow rate is 1ml per minute; the detection wavelength is 245nm.
[0066] Preparation of stationary phase
[0067] Soak 8g of silica gel in 3mol / L hydrochloric acid, heat and reflux for 10h, then wash with double distilled water until neutral, wash with acetone three times, bake at 150°C to remove water and activate for 8h, cool and store ...
Embodiment 2
[0070] (1) Weigh 10 g of Chinese herbal decoction pieces Fructus Aurantii, pulverize with a pulverizer, add 1 L of methanol solvent of analytical grade, and extract by heating to reflux to obtain a crude extract.
[0071] (2) Take 3 g of the crude extract in step (1), add 300 mL of methanol, ultrasonicate, and filter to obtain a filtrate.
[0072] (3) Agilent 1200HPLC high performance liquid chromatography was used to separate the filtrate prepared in step (2).
[0073] The stationary phase is chitosan-modified silica gel filler; the mobile phase is formic acid solution, the molar concentration is 0.4%, and the volume ratio with methanol is 80:20, the flow rate is 1ml per minute; the detection wavelength is 250nm.
[0074] Preparation of stationary phase
[0075] Soak 8g of silica gel in 3mol / L hydrochloric acid, heat and reflux for 10h, then wash with double distilled water until neutral, wash with acetone three times, bake at 150°C to remove water and activate for 8h, cool ...
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