Ultrasound-assisted extraction method of flavonoid compounds in citrus peel
A technology of ultrasonic-assisted extraction and flavonoids, which is applied in the direction of drug combination, pharmaceutical formula, plant raw materials, etc., can solve the problems of weakness and inability to fully realize the high-value utilization of citrus by-products, and achieve the maintenance of healthy stability and high in vitro Antioxidant activity, effect of improving utilization rate
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Embodiment 1
[0085] Embodiment 1: Ultrasonic extraction of citrus peel flavonoids
[0086] (1) Dry the fresh citrus peel at 40°C for 48 hours, crush it through a 40-mesh sieve, pour it into a glass petri dish, seal it with a layer of plastic wrap, and use a 1mL sterile syringe needle to pierce the plastic wrap 3 to 4 times Small holes allow moisture to escape during freeze-drying. After pre-freezing in a -80°C refrigerator for 6 hours, freeze-dry for 24 hours with a vacuum freeze-drying machine. Plate temperature was 5° C., dried for 10 hours, and vacuum degree was 0.01 mbar; freeze-dried citrus peel powder was obtained (stored in a -80° C. refrigerator for later use).
[0087] (2), in a 100mL round-bottomed flask, weigh 1 g of the freeze-dried citrus peel powder obtained in step (1), and add 52% (volume %) ethanol with a solid-liquid ratio of 1:42 (g:mL) Solution 42mL, ultrasonic-assisted extraction: power 325W, ultrasonic time 17min.
[0088] After the extraction, centrifuge at a spee...
Embodiment 2
[0091] Embodiment 2: Macroporous resin purifies citrus peel flavonoids:
[0092] The crude extract of flavonoids of the citrus peel of 14 kinds of oranges obtained in Example 1 is carried out as follows respectively:
[0093] (1), the flavone crude extract is concentrated to 1 / 8 of the original volume, and 95% (volume %) ethanol solution is added to redissolve to the original volume of the flavone crude extract of citrus peel;
[0094] So that the ethanol concentration in the crude extract after reconstitution is higher than 80% (about 85%), place it at 4°C for 12 hours, discard the precipitate, take the supernatant, and use a rotary evaporator to concentrate the supernatant until it has no alcohol smell , to obtain the flavone crude extract after pretreatment; rotary evaporation concentration conditions: water bath temperature 50 ° C, pressure 60 ± 5mbar, rotation speed 50rpm.
[0095] (2), select and weigh 10.00g of non-polar XAD-16 macroporous resin (specific surface area ...
Embodiment 3
[0102] Example 3: Determination of the total content of flavonoids in citrus peel and the components of flavonoids
[0103] (1) Weigh 2 mg of rutin standard substance, transfer it to a 10 mL volumetric flask, add 70% ethanol solution to constant volume, and obtain a 200 μg / mL standard solution. Dilute it into a series of standard solutions with different mass concentrations within the range of 3.125 μg / mL to 100 μg / mL, and perform the following operations on the series of standard solutions:
[0104] Take 1mL of series standard solutions in a 10mL colorimetric tube, add 1mL of 60% (volume %) ethanol solution, and then add 0.3mL of sodium nitrite solution with a mass concentration of 0.05g / mL (weigh 5g of sodium nitrite and add it to a 100mL volumetric flask , then use ultrapure water to make up to 100mL), shake and mix, react for 6min, add 0.3mL of aluminum nitrate solution with a mass concentration of 0.10g / mL (weigh 10g of sodium nitrite and add it to a 100mL volumetric flas...
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