Celangulin TC, its preparation method and quality detection method
A quality detection method and the technology of picolin, applied in the field of botanical pesticides
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[0092] 1. The preparation method of the former medicine of picroderm and emulsion in water
[0093] (1) 35% bitter bark vine raw medicine
[0094] Weigh the shade-dried bitter vine root or / and bark and crush it (pass through a 10-24 mesh sieve), add 2-6 times the volume, 90-95% ethanol, reflux or ultrasonically extract 2-3 times at 60-80°C , extracted for 1-2 hours each time, combined the filtrate after filtration, concentrated under reduced pressure; took the concentrated filtrate (density 0.90-1.19), packed it into a column with 1-2 times its weight of macroporous adsorption resin, and successively washed it with 20~25% ethanol, 40~50% ethanol, 75%~85% ethanol and 90~95% ethanol were washed into the column, and the 75%~85% ethanol eluate was collected, and evaporated to dryness under reduced pressure to obtain the original phalloidin medicine. The model of the macroporous adsorption resin is HP-20, D-101, D-201 or SP-70; the diameter-to-height ratio of the macroporous adso...
Embodiment 1
[0247] (1) Preparation method of 35% T9 picrodermin original drug A
[0248] After sieving, the root and bark of Phyllostachys chinensis that meet the requirements (24 meshes) are sequentially added to ethanol with a volume of 3:2:2 times and a mass ratio of 95%, and reflux extraction at 80°C for 3 times, each time for 2 hours, Filtrate, combine the three filtrates, and concentrate under reduced pressure to a filtrate with a density of 0.95. Get the filtrate, use its weight as 1 times the amount of HP20 resin packing column (diameter-height ratio: 10:1), successively wash the column with 20% ethanol, 40% ethanol, 80% ethanol and 95% ethanol (the ethanol for punching the column 25, 30, 40 and 20 times the volume of the filtrate after concentration respectively), collect the 80% ethanol eluate, evaporate to dryness under reduced pressure, and obtain 35% T9 picroderine original drug A.
[0249]
[0250] (2) 35%T9 picrodermin original drug A quality testing method
[0251] ①P...
Embodiment 2
[0268] (1) The preparation method of 35% T9 picrodermin original drug B
[0269] After sieving, the roots and bark of the bitter vine that meet the requirements (24 meshes) are sequentially added to ethanol with a volume of 3:3:3 times and a mass ratio of 95%, and reflux extraction at 60°C for 3 times, each extraction for 1.5h , filtered, combined three filtrates, and concentrated under reduced pressure to a filtrate with a density of 1.09. Take the filtrate, pack it into a column (diameter-to-height ratio: 10:1) with twice its weight of D-101 resin, and successively wash the column with 25% ethanol, 50% ethanol, 85% ethanol and 90% ethanol (punch the column 25, 30, 40 and 20 times the volume of the ethanol after concentrating the filtrate respectively), collect the 85% ethanol eluate, and evaporate to dryness under reduced pressure to obtain 35% T9 pharethin original drug B.
[0270]
[0271] (2) 35%T9 phatericin original drug B quality detection method
[0272] ①Prepara...
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