Ainsliaea fragrans extract and active component thereof as well as their quality control method
A quality control method and technology of Xingxiang rabbit ear wind, applied in the directions of medical preparations containing active ingredients, preparation of organic compounds, plant/algae/fungus/moss components, etc., can solve the chemical composition and Insufficient pharmacological research, unclear research on active ingredients, etc.
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Embodiment 1
[0047] Example 1: Preparation of Apricot Fragrant Rabbit Ear Wind Extract
[0048] Weigh 1 kg of apricot rabbit ear wind medicinal material, heat and decoct 3 times with 20 times the amount of water (8 times, 6 times, 6 times, soak for half an hour before the first decoction), decoct for 1 hour each time, filter, and the filtrate Combine and concentrate to an amount equivalent to 1g of medicinal material per 1ml (concentration temperature 65-70°C). AB-8 macroporous resin (column bed volume about 5L) was applied to the concentrated solution, and the sample was placed for 4 hours to allow the adsorption to balance. First, it was eluted with distilled water until the eluent was basically colorless, and then eluted with 95% medical alcohol (about 20L), collect the ethanol eluent, concentrate, and dry to obtain about 70g (extraction) of Xingxiang rabbit ear wind extract.
Embodiment 2
[0049] Embodiment 2: Separation and purification of compound 1-6
[0050] Part of the apricot rabbit ear wind extract (about 60g) obtained in Example 1 was added to the silica gel to mix the sample at about 1:3, and the column chromatography under reduced pressure (thin-layer chromatography silica gel H, chemically pure, 250g), followed by With 4000ml of chloroform, 1500ml of chloroform-methanol (3:1), 1500ml of methanol, and 3000ml of methanol-formic acid (95:5) for elution, the eluted parts of each ratio were collected and evaporated to dryness to obtain 1.9g of chloroform-eluted part, chloroform-formic acid (95:5) Methanol (3:1) eluted fraction 16.8g (T3-2) and methanol and methanol-formic acid (95:5) eluted fraction 24.6g. Medium-pressure column chromatography on T3-2 (49mm×230mm, TLC 2 analysis of silica gel H about 200g), followed by elution with different ratios of chloroform-methanol (99:1-65:35, pure methanol) to obtain leaching Cream T3-2-1~T3-2-10 has a total of 10...
Embodiment 3
[0056] Embodiment 3: the quality control method of apricot rabbit's ear wind extract
[0057] Preparation of the test solution: Get 50.5 mg of the obtained Apricot Fragrant Rabbit Earwind extract (extract) in Example 1 and put in a 10ml volumetric flask, add methanol to constant volume, and make fully dissolved to obtain the test solution above ultrasonic 10min. Store in the refrigerator until ready to use.
[0058] Preparation of the reference substance solution: Weigh 10.80 mg of compound 5 into a 10 ml volumetric flask, add methanol to constant volume, and shake well to obtain the reference substance solution C5-h1. Precisely measure C5-h12.000ml and add methanol to a 5ml volumetric flask to obtain the reference substance solution C5-h0.4, precisely measure C5-h11.000ml and add methanol to a 10ml volumetric flask to obtain a reference substance solution C5-h0. 1. Weigh 12.00mg of compound 1 and 25.99mg of compound 8 into the same volumetric flask, add methanol to constant...
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