Extraction method of radix bardanae general flavone

[0020] Example 1

[0021] A method for extracting total flavonoids from burdock root, comprising the following steps:

[0022] Step 1) Clean the fresh burdock root, then heat it in steam at 100°C for 20 minutes, take it out, cool it naturally, cut it into slices with a thickness of 3 mm, then dry it in an oven, pulverize it, and pass it through a 100-mesh sieve to obtain burdock root powder dry powder;

[0023] Step 2) Flatten the dry powder obtained in step 1) into a flat layer with a thickness of 5 mm, and then place it under ultraviolet light for 30 minutes, and the ultraviolet intensity is 3000 mW/cm 2;

[0024] Step 3) Soak the dry powder of step 2) in a 6wt% sucrose solution for 30min, collect the precipitate by centrifugation, and place the precipitate in a cool and ventilated place to dry;

[0025] Step 4) Extract the precipitate obtained in step 3) by refluxing with 75% ethanol for three times, each time for 30 minutes, and the ratio of material to liquid is 1g:10ml, combine the extracts, filter, and collect the filtrate;

[0026] Step 5) Add 1wt% flocculant to the filtrate in step 4), stir evenly, then stand for 40min, filter to remove the precipitate, and collect the supernatant;

[0027] Step 6) Concentrate the supernatant obtained in step 5) under reduced pressure into an extract with a density of 1.2 g/ml, then redissolve with 10 times the mass of purified water, extract twice with chloroform, combine the two aqueous phases, reduce Pressed and concentrated into an extract with a density of 1.3 g/ml, then diluted with twice the weight of purified water, passed through a polyamide column, eluted with 70% ethanol, collected the eluent, evaporated to recover ethanol, and freeze-dried to obtain a precipitate .

[0028] Determination of total flavonoids in the precipitate: Precisely draw 200 μL of the sample solution, place it in a 10 ml volume, measure the absorbance at 510 nm, and calculate the yield of total flavonoids as 24.3 mg/g burdock root dry powder, with a purity of 33.2%.

[0029] The flocculant is prepared according to the following process: (1) Peanut shell powder and sepiolite powder are pulverized to obtain peanut shell powder and sepiolite powder respectively, and peanut shell powder, sepiolite powder and diatomite are obtained by 2:1:1 The mass ratio of diatomite was mixed and stirred evenly, added to a sodium hydroxide solution with a concentration of 1M accounting for 5 times the weight of diatomite, stirred at 200 rpm for 120 min, then filtered, dried, and ground into a powder with a particle size of 10-20 mesh, That is component A; (2) Take chitosan and pectin according to the mass ratio of 10:1, mix and stir evenly, then add 2M sodium hydroxide aqueous solution that accounts for twice the mass of chitosan, ultrasonic at 30KHz for 10min, Finally, stir at 500 rpm for 3 minutes to obtain component B; (3) Mix and stir evenly component A and component B in a mass ratio of 2:1, then place it in a closed reaction kettle, and raise the temperature to a temperature of 2 °C/s. 150 ℃, heat preservation for 30 min, take out, put into a mixer, stir at 500 rpm for 3 min to obtain a mixture, put it in an oven, dry at 80 ℃ for 60 min, take out, and pulverize.

[0030] Example 2

[0031] A method for extracting total flavonoids from burdock root, comprising the following steps:

[0032] Step 1) Clean the fresh burdock root, then place it in 100 ℃ steam for heat treatment for 15 minutes, take it out, cool it naturally, cut it into slices with a thickness of 3 mm, then dry it in an oven, pulverize it, and pass it through a 100-mesh sieve to obtain burdock root powder dry powder;

[0033] Step 2) Flatten the dry powder obtained in step 1) into a flat layer with a thickness of 5mm, and then place it under ultraviolet light for 20 minutes, and the ultraviolet intensity is 3000mW/cm 2;

[0034] Step 3) Soak the dry powder of step 2) in a 6wt% sucrose solution for 30min, collect the precipitate by centrifugation, and place the precipitate in a cool and ventilated place to dry;

[0035] Step 4) Extract the precipitate obtained in step 3) by refluxing with 75% ethanol for three times, each time for 30 minutes, and the ratio of material to liquid is 1g:10ml, combine the extracts, filter, and collect the filtrate;

[0036] Step 5) Add 0.5wt% flocculant to the filtrate in step 4), stir evenly, then stand for 60min, filter to remove the precipitate, and collect the supernatant;

[0037] Step 6) Concentrate the supernatant obtained in step 5) under reduced pressure into an extract with a density of 1.2 g/ml, then redissolve with 10 times the mass of purified water, extract twice with chloroform, combine the two aqueous phases, reduce Pressed and concentrated into an extract with a density of 1.3g/ml, then diluted with twice the weight of purified water, passed through a polyamide column, eluted with 70% ethanol by volume, collected the eluate, evaporated to recover ethanol, and freeze-dried to obtain Precipitate.

[0038] Determination of total flavonoids in the precipitate: Precisely draw 200 μL of the sample solution, place it in a 10 ml volume, measure the absorbance at 510 nm, and calculate the yield of total flavonoids to be 23.9 mg/g burdock root dry powder, with a purity of 32.7%.

[0039]The flocculant is prepared according to the following process: (1) Peanut shell powder and sepiolite powder are pulverized to obtain peanut shell powder and sepiolite powder respectively, and peanut shell powder, sepiolite powder and diatomite are obtained by 2:1:1 The mass ratio of diatomite was mixed and stirred evenly, added to a sodium hydroxide solution with a concentration of 1M accounting for 5 times the weight of diatomite, stirred at 200 rpm for 120 min, then filtered, dried, and ground into a powder with a particle size of 10-20 mesh, That is component A; (2) Take chitosan and pectin according to the mass ratio of 10:1, mix and stir evenly, then add 2M sodium hydroxide aqueous solution that accounts for twice the mass of chitosan, ultrasonic at 30KHz for 10min, Finally, stir at 500 rpm for 3 minutes to obtain component B; (3) Mix and stir evenly component A and component B in a mass ratio of 2:1, then place it in a closed reaction kettle, and raise the temperature to a temperature of 2 °C/s. 150 ℃, heat preservation for 30 min, take out, put into a mixer, stir at 500 rpm for 3 min to obtain a mixture, put it in an oven, dry at 80 ℃ for 60 min, take out, and pulverize.

[0040] Example 3

[0041] Take the process of Example 1 as an example to detect the influence of each parameter and condition on the extraction efficiency:

[0042] Groups: control group 1, control group 2, example group 1;

[0043] Control group 1: do not use sucrose soaking and ultraviolet irradiation, other is the same as Example 1;

[0044] Control group 2: not treated with flocculant, treated with activated carbon, the others are the same as in Example 1.

[0045] The determination of total flavonoids in the precipitate is shown in Table 1:

[0046] Table 1

[0047] group Contentmg/g burdock root dry powder purity% Example 1 24.3 33.2 control group 1 14.6 29.7 control group 2 20.8 21.8