Extract the preparation method of Hesperidin Solgar from 4 tons of Citrus aurantium, it comprises the following steps:
(1) After weighing 4 tons of Fructus Citrus Fructus Fructus Fructus Fructus Powder, pour into the extraction tank, and arrange and level off;
(2) preparation raw material is the alkaline solution of 4 times of Fructus Aurantii fine powder, and the density of sodium carbonate in this alkaline solution is got 2kg/m3, and the density of 30% liquid caustic soda is 1.5kg/m3, this alkaline solution is piped from tank bottom Pump it into the extraction tank, and when the solution is exposed to the material surface, change the liquid from the fence coil until the liquid is pumped; after 1.5 hours of dynamic immersion, drain the liquid in the extraction tank; Turn it over once and shake the bottom fence to loosen the fine powder on the fence surface;
(3) Prepare 4 times the alkali solution of the raw material, the density of sodium carbonate in this alkali solution is 1.5kg/m3, the density of 30% liquid caustic soda is 0.5kg/m3, this alkali solution is pumped into the extraction tank from the tank bottom coil pipe , when the solution is exposed to the surface of the material, enter the liquid from the bottom coil until the liquid is pumped; open the steam valve to feed steam into the bottom and middle of the tank for boiling; after boiling, adjust the upper and lower steam valves according to the data of the steam pressure gauge Keep boiling in the tank for 30 minutes, close the steam valve, and drain the cooking liquid at 15m3/h;
(4) prepare 25 times of alkaline solution of raw material, the density of sodium carbonate in this alkaline solution is 1.5kg/m3, the density of 30% liquid caustic soda is 0.5kg/m3, treat that the boiling liquid of step (3) is discharged to material and expose At the liquid level, inject the alkaline solution into the tank from the material level for percolation treatment, and control the liquid flow rate to 3.8m 3 /h; stop the liquid after processing 10 times the liquid, and filter the liquid in the tank; Material method Turn the material in the tank thoroughly once, and shake the bottom fence to loosen the fine powder on the fence surface;
(5) inject the used remaining alkaline solution of step (4) from the bottom to the solution just to expose the material surface, use density instead as 2kg/m The sodium carbonate solution injects in the tank from the material surface and carries out the second diafiltration process, and control The liquid flow rate is 3.8m3/h, and the diafiltration treatment is that when the filtrate is added with hydrochloric acid to adjust the pH to between 3 and 4, the treatment is qualified, and the period of the diafiltration treatment is not less than 15 hours; After the inner liquid has percolated, turn the material in the tank thoroughly again;
(6) 25 times the hesperidin extract of the configuration raw material, the hesperidin extract is a sodium hydroxide solution, the density of sodium hydroxide in the solution is 13kg/m3, the Hesperidin Solgar extract is pumped into the extraction tank for Extract hesperidin and collect the excreted liquid. The extraction period is 15 hours;
(7) Adjust the pH value of the discharge liquid of step (6) to between 5 and 6 with hydrochloric acid, and stir the discharge liquid until hesperidin is precipitated;
(8) After the solution treated in step (7) was left to stand for 2 hours, the clear solution above was taken out, and the remaining crystal solution was pumped into the plate and frame machine to filter and dried, and then put into a drying room for drying. That is to obtain 460kg of Hesperidin Solgar with a purity of 90%-95%.
A kind of extraction process of Hesperidin Solgar:
S1. Preparation of alcohol solution: 5 parts of methanol, 2 parts of ethanol and 1 part of isobutanol were mixed to prepare an alcohol solution.
S2, pulverization: first select the Citrus aurantium Fructus that contains 5.61% hesperidin as raw material, and raw material consumption is 100kg, then raw material is carried out ultra-high pressure gas explosion, and the pressure that ultra-high pressure gas explosion adopts is 60MPa.
S3. Extraction: Under the condition of 80°C, the raw material and the strong alkali solution were mixed and reacted for 5 minutes for degumming treatment, wherein the concentration of the strong alkali solution was 8mol/L, and the raw material and the strong alkali solution were mixed according to the ratio of 12mL per gram of raw material Strong base solution ratio for mixing. After degumming is completed, under the condition of 60 ℃, add alcoholic solution, at this moment, every 100mL solution contains 1 gram of raw material in the mixture obtained after raw material, strong alkali solution and alcoholic solution are mixed. After mixing, adopt high-speed homogenization method to carry out supercritical fluid extraction, wherein the rotating speed of high-speed homogenization method is 700 rpm. The pressure of the supercritical fluid extraction is 20MPa, the temperature is 50°C, the entrainer is acetone, and the flow rate of carbon dioxide is 15L/min. Simultaneously, the mixture was sonicated at a frequency of 30KHz. The extraction time was 4 hours.
S4, purification: the extract obtained by extraction is filtered to obtain the filtrate, and then quantum resonance molecular collision is carried out for 30 minutes. Among them, the temperature in the quantum resonance molecular collision ion reactor is first raised from 0°C to 47°C and then lowered from 47°C to 0°C. , and then the filtrate is concentrated again, and the multiple of concentration is 5 times. After concentrating, adopt DM130 type macroporous adsorption resin to carry out further purification, the flow rate of concentrated solution is 1.3mL/min, and the scope of pH value is then 10.4, and eluent is the mixed solution of 30% ethanol and 72% methanol, and 30% The ratio of % ethanol and 72% methanol is 1:4. After the elution was completed, the pH value was adjusted with dilute hydrochloric acid so that the pH value of the eluent was 3.2, and finally filtered and dried to obtain 4.49Kg of hesperidin, the purity of Hesperidin Solgar was 98.3%, and the extraction efficiency was 80.0%.
Choose Citrus aurantium with a synephrine content of 1.34% and a Hesperidin Solgar content of 4.94%, dry it and crush it to below 10 mesh, weigh 100kg, add 400L of petroleum ether to mix, reflux at 70°C for 40min, and filter with a ceramic membrane Once, the filtrate was obtained, and then concentrated under reduced pressure to remove petroleum ether to obtain the essential oil of Citrus aurantium. Mix Citrus aurantium filter residue with 250L of 20% ethanol aqueous solution, wherein the ethanol aqueous solution also contains 0.0001mol/L NaOH, mix, reflux and extract at 45°C for 40min, filter once with a ceramic membrane to obtain filtrate, repeat once more, combine filtrate to obtain 400L of mixed extract. Concentrate the extract to obtain 50L concentrated solution I, which is adsorbed on KLFC-150 macroporous resin, and contains 40% ethanol, 0.001mol/LNaOH ethanol aqueous solution for elution to obtain 120L eluent I, and The eluent I was concentrated under reduced pressure at 50°C to 15 L to obtain the concentrated solution II. Then use ethanol aqueous solution containing 60% ethanol and 0.0001mol/L NaOH to elute KLFC-150 macroporous resin to obtain 200L eluent II, and concentrate the eluent II under reduced pressure at 50°C to 20L to obtain concentrated Liquid III. Use 0.01mol/L hydrochloric acid solution to adjust the pH of the concentrated solution II to about 7.5, let it stand at 4°C overnight for crystallization, and filter it once with a ceramic membrane to obtain the crystallization product, which is 0.885 kg of synephrine sample. Use 0.01mol/L hydrochloric acid solution to adjust the pH of the concentrated solution III to about 6, let it stand at 4°C overnight for crystallization, and filter it once with a ceramic membrane to obtain the crystallization product, which is 3.65kg of hesperidin sample. Detection equipment is Agilent1100 high-performance liquid chromatograph, and chromatographic column is Hypersil ODS (250mm * 4.6mm, 5 μ), the detection condition of hesperidin: mobile phase is water: acetonitrile: acetic acid solution (80:16:4, V/ V), the detection wavelength is 280nm, the flow rate is 1 ml/min, and the injection volume is 20 μL; the liquid chromatography detection conditions of synephrine: mobile phase is acetonitrile: water: 0.1% sodium hydroxide solution (32:68:0.2 , V/V), the detection wavelength was 22 5nm, the flow rate was 1 ml/min, and the injection volume was 20 μL. The purity of the Hesperidin Solgar sample is 95.54%, and the product yield reaches more than 70%. The purity of the synephrine sample is 97.25%, and the product yield reaches more than 60%.
