Process of preparing high purity chlorogenic acid and flavonid with eucommia leaf
A technology of chlorogenic acid and Eucommia leaves, which is applied in the field of preparation of high-purity chlorogenic acid and total flavonoids, can solve the problems of many kinds of reagents, cumbersome process, and large solvent consumption, and achieve high target component content and process flow The effect of simplicity and stable product quality
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Embodiment 1
[0032] The selection of embodiment 1 extraction process condition:
[0033] (1) Effect of pulverized Eucommia leaves on the extraction rate of chlorogenic acid and total flavonoids
[0034] Eucommia leaves
extract
(kg)
total flavonoids
Extract contains
quantity(%)
Chlorogenic acid
mass (g)
Extraction rate
(%)
Extract contains
quantity(%)
total flavonoids
amount (g)
Extraction rate
(%)
Original leaf
medium powder
1.02
0.94
0.92
0.95
8.53
11.25
11.36
11.28
80.0
105.7
104.5
107.2
69.26
91.56
90.49
92.78
21.87
30.55
31.19
30.48
223.1
287.2
286.9
289.6
70.26
90.45
90.38
91.21
[0035] It can be seen from the above table that pulverizing Eucommia leaves increases the contact area between the ra...
Embodiment 2
[0046] The selection of embodiment 2 separation process
[0047] (1) The influence of the choice of macroporous resin type on the separation effect
[0048] Experimental method: Extract 5kg of eucommia leaf coarse powder with 45% ethanol solution with pH=4 at 70°C for 1.5 hours each time, concentrate the combined extracts to 4L and centrifuge, and take the supernatant as eucommia leaf The extract was determined to have a dry weight of 0.9kg, a mass content of chlorogenic acid of 11.3% and a mass content of total flavonoids of 30.5%. The extract was divided into 7 parts on average, and the macroporous resin was used for static saturated adsorption, and the adsorption capacity and desorption rate of different types of resins for chlorogenic acid and total flavonoids were calculated respectively. Macroporous resin mainly selects non-polar resin XDA-5, LSA-20, D140, polar resin NKA-II, HPD-400, HPD-400A and medium polar resin JD-1 in the method of the present invention.
[0049]...
Embodiment 3
[0053] The process selection of embodiment 3 chlorogenic acid refining process
[0054] (1) The effect of the amount of silica gel on the separation of chlorogenic acid silica gel column
[0055] Crude chlorogenic acid
[0056] (2) The effect of mobile phase on the separation of chlorogenic acid silica gel column
[0057] Experimental method: take 0.25kg of crude chlorogenic acid (content is 24.5%) and dissolve it in 100ml of methanol, mix the sample with 125g of silica gel and put it on a silica gel column, elute with eluent, collect in sections, concentrate under reduced pressure, and collect in sections The fractions were monitored by HPLC, and fractions with a content higher than 90% were combined and concentrated to dryness. The results showed that ethanol, acetone, ethyl acetate and methanol were selected as eluents, and the recovery rate of chlorogenic acid was above 85%, and the effect of ethyl acetate was the best. Although the elution effect of ethyl acet...
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