Extracting and purifying technology for haw flavonoids substances
A technology of hawthorn extract and total flavonoids, applied in medical preparations containing active ingredients, plant/algae/fungus/moss components, plant raw materials, etc., can solve the comprehensive and systematic research on the extraction and purification process of hawthorn total flavonoids that have not been seen, etc. problem, to achieve the effect of shortening the heating time, high transfer rate and preventing clogging
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Embodiment 1
[0028] Example 1 Extraction process experiment of hawthorn total flavonoids
[0029] (1) use the ethanol reflux extraction method to carry out the experiment, adopt L 9 (3 4 ) Orthogonal experimental method to investigate the process parameters of ethanol concentration, ethanol dosage (multiple of hawthorn weight), extraction time and particle size of decoction pieces in ethanol reflux extraction of total flavonoids in hawthorn, and adopt ultraviolet-visible spectrophotometry to analyze the total flavonoids in the extract. The content was measured and used as an index for comparative analysis. The results are shown in Table 1, Table 2 and Table 3.
[0030] Table 1 Level table of experimental factors
[0031]
Level
factor
A
Ethanol concentration (%)
B
Ethanol consumption (multiple)
C
time (hours)
D.
Particle size
1
2
3
60
70
80
...
Embodiment 2
[0039] Example 2 Macroporous resin purification process experiment of hawthorn total flavonoids
[0040] The hawthorn extract that extracts with aforementioned optimal extraction condition is carried out following experiment:
[0041] (1) Screening experiment of macroporous resin
[0042] Resin source: D101 resin (Tianjin Haiguang Chemical Co., Ltd.), AB-8, D4020 resin (Nankai University Chemical Plant), SP825, HP20, SP70 (Japan Mitsubishi Corporation).
[0043] The screening results of the resin are shown in Table 4, Table 5, and Table 6.
[0044] Table 4 Determination results of static saturated adsorption capacity of five resins
[0045] Resin type
polarity
Hawthorn total flavonoid adsorption (mg)
D-101
AB-8
SP825
HP20
D4020
non-polar
weak polarity
non-polar
non-polar
non-polar
11.37
11.09
11.42
7.48
5.87
[0046] Table 5 Desorption measu...
Embodiment 3
[0077] Embodiment 3 Pilot scale scale-up experiment
[0078] Weigh 15 kg of hawthorn decoction pieces, reflux extraction with 70% ethanol for 3 times, use 120 liters of ethanol for the first time, reflux extraction for 2 hours, use 90 liters of ethanol for the second and third times, reflux extraction for 1 hour respectively, and combine the extracts for 3 times , recover the ethanol until it has no alcohol smell, let it stand overnight, filter the precipitate with a filter cloth the next day, dilute to a solution containing 0.1 g of crude drug per ml, and set aside.
[0079] Soak 20 kg of pharmaceutical grade D101 macroporous resin with an appropriate amount of ethanol, put it on the column by wet method, and treat it for later use.
[0080] The extracted medicinal solution was loaded into the resin column twice, 75 liters each time, the flow rate of the sample was 2 times the column volume / hour, and the pH value was the pH value of the original medicinal solution (about pH 3...
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