CN109293721B - Method for preparing neohesperidin in physiological pomelo fruit drops by using alcohol/salt aqueous two-phase system - Google Patents
Method for preparing neohesperidin in physiological pomelo fruit drops by using alcohol/salt aqueous two-phase system Download PDFInfo
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Abstract
The invention belongs to the technical field of plant component extraction and discloses a method for preparing neohesperidin in physiological pomelo fruit drops by an alcohol/salt aqueous two-phase system, which comprises the following steps: collecting physiological fruit drops of the dried grapefruit; crushing; crushing; preparing and constructing a two-water-phase system; hot dipping extraction; separating and phase-splitting the liquid-solid three-phase disc separator; concentrating; water is precipitated and crystallized and is filtered; carrying out hot water recrystallization purification with the assistance of an ultrafiltration membrane; cooling and crystallizing; and (5) drying and packaging. The invention adopts isopropanol/NaH 2 PO 4 The whole process has the advantages of short production period, mild extraction conditions, simple and convenient operation, high selectivity to target products, good product quality, small amount of wastewater, easy treatment and the like; the yield of the prepared neohesperidin reaches 5.7%, and the HPLC content is more than or equal to 95%.
Description
Technical Field
The invention particularly relates to a method for preparing neohesperidin in physiological pomelo fruit drops by using an alcohol/salt aqueous two-phase system, and belongs to the technical field of plant component extraction.
Background
Neohesperidin is flavone extracted from natural orange, grapefruit, etc. Neohesperidin (Neohesperidin) is a flavanone compound, and structural analysis shows that Neohesperidin is glucoside consisting of two units, namely glucoside ligand 3,5, 7-trihydroxy-4' -methoxyflavone and glycosyl ligand rhamnosyl beta-1, 2-glucose. Because neohesperidin has the activities of scavenging free radicals, promoting gastric motility, reducing blood fat, resisting atherosclerosis, protecting nervous system, resisting allergy, resisting cancer and the like, the neohesperidin has wide application in the aspect of medicine; neohesperidin is also an important intermediate, can be converted into Neohesperidin Dihydrochalcone (Neohesperidin Dihydrochalcone) which is a derivative thereof under certain conditions, and the compound is a safe low-calorie sweetener (the sweetness is 1500-1800 times that of cane sugar), a bitter taste inhibitor and a flavor blender, has good thermal stability and wide application pH range, and is extremely widely applied in the industries of food, beverage, pharmacy and animal feed. This finding has led to a rapid expansion of the use and application range of neohesperidin. Because some Rutaceae plants such as lime, sweet orange, pomelo, immature bitter orange, bitter orange and radix zanthoxyli contain neohesperidin, the traditional plant extraction method is the main method for preparing neohesperidin, and the chemical synthesis method of naringin is adopted. There are many disadvantages in the production process. The problems existing in the extraction process of the prior art are mainly as follows:
(1) When the Rutaceae plants are used as raw materials to extract neohesperidin, methanol or ethanol is mostly adopted for hot reflux extraction, the temperature reaches more than 85 ℃, and a large amount of flavonoid substances such as naringin, hesperidin and the like are dissolved out in the extraction process, so that the purity of the neohesperidin is seriously influenced, and the difficulty and the cost of a subsequent purification process are greatly improved;
(2) In the extraction process, a multifunctional extraction tank is used for reflux extraction, a percolation mode is required during extraction, the alcohol content of the medicine residues is extremely high after extraction is finished, great solvent waste is caused, and the medicine residues containing alcohol are also important hazard sources.
(3) In the extraction process, a large amount of steam is needed for heating, the danger coefficient is high, the energy consumption is high, and the production cost is high.
(4) In the preparation process of chemically synthesizing neohesperidin from naringin, naringin needs to be hydrolyzed by using a strong alkaline solution, and then the hydrolysate is condensed with isovanillin aldol to generate the neohesperidin. The strong alkaline waste water produced in the production process causes great environmental pollution, and a large amount of isovanillin is needed as a reactant to ensure the conversion rate of naringin, thereby increasing the production cost.
Disclosure of Invention
The invention aims to solve the technical problems and overcome the existing defects, provides a method for preparing neohesperidin in physiological pomelo fruit drops by using an alcohol/salt aqueous two-phase system, has the advantages of high selectivity, mild conditions, simple process, convenience in operation, environmental friendliness and high efficiency, and can effectively solve the problems in the background art.
In order to solve the technical problems, the invention provides the following technical scheme:
the invention provides a method for preparing neohesperidin in pomelo physiological fallen fruits from pomelo in an alcohol/salt aqueous two-phase system, which comprises the following steps:
s1, collecting the physiological fallen fruits of the dried pomelo: the physiological fruit dropping of the pomelo or the artificial fruit dropping, and the sun drying or the oven drying are carried out, so that the raw materials are stably supplied during the industrial production;
s2, crushing and grinding: crushing a certain mass of dried pomelo physiological fruit drop or artificial fruit thinning fruit drop in a hammer crusher, and grinding crushed coarse particles into powder by a wood flour machine to obtain dried pomelo fruit powder; the preferable dry grapefruit powder is 100-300 meshes, and the fine dry grapefruit powder can ensure high extraction rate and short extraction time;
s3, preparing and constructing a double water phase system: adding deionized water in an amount which is 3 to 5 times the weight of the dried pomelo powder into a liquid preparation tank, and weighing food-grade NaH with a certain weight 2 PO 4 Inorganic salt (GB 25564-2010) is fully stirred and dissolved to prepare NaH with the mass fraction of 20% 2 PO 4 Fully dissolving the solution, measuring 70 percent isopropanol with the same volume to construct isopropanol/NaH with certain mass 2 PO 4 Inorganic salt aqueous two-phase system, ph = 4-5.5. The isopropanol/NaH 2 PO 4 The inorganic salt aqueous two-phase system can effectively ensure extraction of neohesperidin from the physiological fruit drop of the pomelo, and simultaneously reduce dissolution of other flavonoid substances such as the naringin, the hesperidin and the like, thereby achieving the effect of high selectivity on the neohesperidin in the extraction process;
s4, hot dipping extraction: pumping the aqueous two-phase system in the step S3 into an extraction tank, adding the dried pomelo powder in the step S2, starting a machine to stir, controlling the rotating speed to be 50-80 r/min, carrying out hot reflux extraction for 2-3 h, and controlling the temperature to be 50-60 ℃; the preferable extraction tank is dynamic immersion extraction equipment, and the shaddock dry powder and the isopropanol/NaH are fully stirred in a strong mechanical mode 2 PO 4 Inorganic salt is fused in a two-aqueous phase system, so that the aim of fully extracting the neohesperidin is fulfilled; the extraction temperature is preferably 50-60 ℃, and the solubility of naringin and hesperidin is low at the temperature, so that the dissolution of impurities such as naringin and hesperidin is controlled;
s5, separating and phase-splitting a liquid-solid three-phase disc separator: pumping the extracted material into a liquid-solid three-phase disc separator by a screw pump for separating and phase splitting, controlling the feeding speed to be 2-5 cubic/h, separating to obtain a solid phase, a light phase liquid (upper phase liquid) and a heavy phase liquid (lower phase liquid), and enriching the neohesperidin into the upper phase (isopropanol); the preferable separation factor of the liquid-solid three-phase disc separator is 6000-7000, and the liquid-solid three-phase disc separator mainly comprises an inlet and outlet device, a rotary drum, a vertical shaft, a transverse shaft, a machine body, a speed measuring device, a brake device, a motor and the like, wherein the motor drives the rotary drum to rotate at a high speed around a main shaft through a clutch helical gear pair. The disc rack in the rotary drum is filled with discs, so that the equivalent sedimentation area is fully increased, and the feed liquid flows to the bottom of the rotary drum from the upper central feeding pipe. The flow-dividing hole passing through the lower surface of the disk seat is toward the rotary drum wall. Under a centrifugal force field, solid-phase matters heavier than liquid are deposited on the wall of a rotary drum to form sediment, the sediment is discharged from the rotary drum through a slag discharge mechanism under the condition of no shutdown, light liquid flows to an upper light liquid centripetal pump along the outer (upper) conical surface of a conical disc towards the axis and is discharged from a light liquid outlet, heavy liquid flows upwards to the wall of the rotary drum along the inner (lower) conical surface of the disc, then flows upwards through the heavy liquid centripetal pump and is discharged from the heavy liquid outlet, and finally the purpose of separating liquid from liquid to solid is achieved;
s6, concentration: taking the upper phase liquid, concentrating the upper phase liquid by 3 to 5 times in a single-effect falling-film evaporator at the temperature of between 65 and 75 ℃ to obtain a concentrated solution, wherein the baume degree is 3 to 8 degrees Be;
s7, water precipitation crystallization and filtration: taking the concentrated solution, cooling to normal temperature, and mixing the concentrated solution according to the total weight of the concentrated solution of 1: 1-1.2 times of deionized water is added, and after uniform stirring, standing and crystallizing for 5 hours; filtering with a box filter press to obtain a neohesperidin crude product; the chamber filter press preferably uses 3927 type filter cloth;
s8, ultrafiltration membrane assisted hot water recrystallization purification: putting all the crude neohesperidin in S7 into a liquid preparation tank, adding 8-10 times of deionized water, heating to 80-85 ℃, stirring for 1-2 hours to fully dissolve the neohesperidin, filtering out insoluble suspended matters by using a hollow fiber membrane, obtaining clear filtrate at the pressure of 1.2-1.5 bar and the filtering speed of 500-600L/h, and performing ultrafiltration on the clear filtrate by using a GE4040 type 3500 Dalton ultrafiltration membrane at the pressure of 20-25 bar and the filtering speed of 500-600L/h to obtain refined extract; the hollow fiber membrane is preferably a 50-nanometer tubular membrane, and the ultrafiltration membrane is preferably a 3500-Dalton tubular membrane;
s9, cooling and crystallizing: cooling and crystallizing the refined extract in the S8 in a crystallization tank for 5-8 h at 10-15 ℃, stirring at 5-10 r/min, and filtering by a three-leg centrifuge to obtain a filter cake, wherein the three-leg centrifuge preferably uses 750A type filter cloth;
s10: and (3) drying and packaging: and (S9) drying the filtered filter cake for 5-8 h at 80-85 ℃ under reduced pressure by using a rake dryer, determining that the drying end point is when the moisture content is detected to be less than 5%, packaging and warehousing to obtain a finished product of neohesperidin, wherein the HPLC content is more than or equal to 95%.
The method selects the physiological fruit dropping of the pomelo or the artificial fruit dropping, and the dried or dried pomelo, wherein the Chinese is a great planting country of the pomelo, a large amount of the physiological fruit dropping of the pomelo is provided every year, the raw materials are sufficient and cheap, and the dried pomelo has the advantages of convenient transportation, easy storage and the like.
The invention grinds the crushed and crushed pomelo fruits which are fallen physiologically or thinned artificially and dried, saves the extraction time, milds the extraction conditions and improves the extraction yield.
The invention adopts isopropanol/NaH for extraction 2 PO 4 The inorganic salt aqueous two-phase system can effectively ensure extraction of neohesperidin from the physiological fruit drop of the pomelo, and simultaneously reduce dissolution of other flavonoid substances such as the naringin, the hesperidin and the like, thereby achieving the effect of high selectivity on the neohesperidin in the extraction process.
The extraction temperature is 50-60 ℃ during extraction, and the solubility of naringin and hesperidin is low at the temperature, so that the dissolution of impurities such as naringin and hesperidin is controlled, the energy is saved, the relative singleness of extracted substances is ensured, and conditions are provided for the high purity of products.
The invention adopts a liquid-solid three-phase disc separator during extraction, and separation factors are 6000-7000, thereby maximally reducing the content of the solvent in the solid phase, ensuring the complete separation of the light phase liquid and the heavy phase liquid, clarifying the light phase liquid, effectively reducing the difficulty of liquid-solid three-phase separation, saving the production cost and shortening the production period.
According to the invention, an ultrafiltration membrane is adopted to assist hot water recrystallization purification during refining, so that the molecular-level impurity removal is realized, impurities such as macromolecular pigments, proteins and pectin are filtered, the purification conditions are mild, the purification steps are reduced, and the purity and color of the product are ensured to the maximum extent.
The invention has the beneficial effects that: in the method provided by the invention, the dried physiological fallen pomelo fruits or artificial sparse fallen pomelo fruits are selected as raw materials, so that the sufficient supply of raw materials for industrial production is ensured. The powder is extracted, so that the product yield is effectively improved; with isopropanol/NaH 2 PO 4 The inorganic salt aqueous two-phase system is used as an extraction solvent, so that the extraction of neohesperidin is ensured, other flavonoid impurities such as naringin, hesperidin and the like are effectively reduced, the selectivity of neohesperidin in the extraction process is ensured, and the extraction rate is improved; the extraction is carried out in a hot dipping (50-60 ℃) mode, the dissolution of impurities such as naringin, hesperidin and the like is further controlled, the energy is saved, the relative singleness of extracted substances is ensured, and conditions are provided for the high purity of the product; by adopting the liquid-solid three-phase disc separator, the content of the solvent in the solid phase is reduced to the maximum extent, the complete separation of light phase liquid and heavy phase liquid is ensured, the light phase liquid is clarified, the difficulty of liquid-solid three-phase separation is greatly reduced, the production cost is saved, and the production period is shortened; the ultrafiltration membrane is adopted to assist hot water recrystallization purification, so that the molecular-level impurity removal is realized, impurities such as macromolecular pigment, protein, pectin and the like are filtered, the purification conditions are mild, the purification steps are reduced, and the purity and color of the product are ensured to the maximum extent; the whole process has the advantages of short production period, mild extraction conditions, simple and convenient operation, high selectivity to target products, good product quality, small amount of waste water, easy treatment and the like; the yield of the prepared neohesperidin reaches 5.7%, and the HPLC content is more than or equal to 95%.
Detailed Description
The following description of the preferred embodiments of the present invention is provided for the purpose of illustration and description, and is in no way intended to limit the invention.
Example 1:
s1, taking 550 kg of dried pomelo physiological fallen fruits, and conveying to a crushing machine room;
s2: crushing and grinding the dried fruits in the S1 to 100-300 meshes by a hammer type grinder and a wood powder machine in sequence, and taking 500kg of the crushed dried fruits for later use;
s3, adding 2 cubic cubes of deionized water into the liquid preparation tank, and weighing 400 kilograms of food gradeNaH 2 PO 4 Inorganic salt is fully stirred and dissolved to ensure that the mass fraction is 20 percent (w/w), after being fully dissolved, 2 cubes of 70 percent isopropanol are measured to construct about 4 cubes of isopropanol/NaH 2 PO 4 Inorganic salt aqueous two-phase system, ph =5.1;
s4, pumping all the aqueous two-phase system in the S3 into an extraction tank, adding 500kg of dried pomelo powder in the S2, starting mechanical stirring, controlling the rotation speed to be 60 r/min, carrying out hot reflux extraction for 2.5h, and controlling the temperature to be 55 ℃;
s5, pumping the extracted material into a liquid-solid three-phase disc separator by using a screw pump to separate and split the phase, controlling the feeding speed to be 2 cubic/h, and separating to obtain a solid phase, a light phase liquid (upper phase liquid) and a heavy phase liquid (lower phase liquid), wherein the neohesperidin is mainly concentrated in the light phase liquid;
s6, pumping the light phase liquid into an evaporation circulating tank, and concentrating the light phase liquid by 5 times in a single-effect falling-film evaporator at 68 ℃ to obtain about 400L of concentrated liquid with a baume degree of 5 DEG Be;
s7, pumping the concentrated solution into a crystallization tank, stirring, cooling to normal temperature, adding 450L of deionized water, stirring uniformly, standing for crystallization for 5 hours, pumping into a box-type filter press, and filtering to obtain 102.5 kg (containing water) of a neohesperidin crude product;
s8, putting 100 kg of neohesperidin crude product in the S7 into a liquid preparation tank, adding 800L of deionized water, heating to 83 ℃, stirring for 1.5h to fully dissolve the neohesperidin crude product, pumping the neohesperidin crude product into a hollow fiber membrane, filtering to remove insoluble suspended matters, filtering at a pressure of 1.5bar and a filtering speed of 520L/h to obtain about 800L of clear filtrate (containing cleaning liquid), and performing ultrafiltration on the clear filtrate (containing cleaning liquid) through a GE4040 type 3500 Dalton ultrafiltration membrane at a pressure of 25bar and a filtering speed of 600L/h to obtain 800L of refined extracting solution (containing cleaning liquid);
s9, cooling and crystallizing 800L of refined extract in the S8 in a crystallizing tank for 6 hours at the temperature of 15 ℃, stirring at the speed of 10 r/min, and filtering by a three-leg centrifuge after crystallization to obtain a filter cake;
s10, drying the filter cake obtained after filtration in the S9 for 8 hours at 85 ℃ under reduced pressure by using a rake dryer, crushing, packaging and warehousing to obtain 28.3kg of finished neohesperidin, wherein the HPLC content is not less than 95%, and the yield is 5.66%.
Example 2:
s1, taking 1080 kg of dried pomelo, and conveying to a crushing machine room;
s2: crushing and grinding the dried fruits in the step S1 to 100-300 meshes by a hammer type crusher and a wood powder machine in sequence, and taking 1000kg of the crushed and ground fruits for later use;
s3, adding 3 cubic cubes of deionized water into the liquid preparation tank, and weighing 600 kilograms of food-grade NaH 2 PO 4 Fully stirring and dissolving inorganic salt to ensure that the mass fraction of the inorganic salt is 20 percent (w/w), weighing 3 cubic 70 percent isopropanol after fully dissolving, and constructing about 10 cubic isopropanol/NaH 2 PO 4 Inorganic salt aqueous two-phase system, ph =4.7;
s4, pumping all the aqueous two-phase system in the S3 into an extraction tank, adding 1000kg of dried pomelo powder in the S2, starting mechanical stirring, controlling the rotating speed to be 65 r/min, carrying out hot reflux extraction for 3h, and controlling the temperature to be 57 ℃;
s5, pumping the extracted material into a liquid-solid three-phase disc separator by using a screw pump to separate and split the phase, controlling the feeding speed to be 5 cubic/h, and separating to obtain a solid phase, a light phase liquid (upper phase liquid) and a heavy phase liquid (lower phase liquid), wherein the neohesperidin is mainly concentrated in the light phase liquid;
s6, pumping the light phase liquid into an evaporation circulating tank, and concentrating the light phase liquid in a single-effect falling-film evaporator at 72 ℃ by 4 times to obtain about 1500L of concentrated liquid with a baume degree of 4.2 degrees Be;
s7, pumping the concentrated solution into a crystallization tank, stirring, cooling to normal temperature, adding 1800L of deionized water, stirring uniformly, standing for crystallization for 5 hours, pumping into a box-type filter press, and filtering to obtain 146.7 kg (containing water) of a neohesperidin crude product;
s8, putting 146.7 kilograms of neohesperidin crude product in the S7 into a liquid preparation tank, adding 1000L of deionized water, heating to 82 ℃, stirring for 1.6 hours to fully dissolve the neohesperidin crude product, pumping the mixture into a hollow fiber membrane to filter and remove insoluble suspended matters, filtering the mixture at a pressure of 1.4bar and a filtering speed of 530L/h to obtain about 1000L of clear filtrate (containing cleaning liquid), and performing ultrafiltration on the clear filtrate (containing cleaning liquid) through a GE4040 type 3500 Dalton ultrafiltration membrane at a pressure of 22bar and a filtering speed of 610L/h to obtain about 1000L of refined extracting solution (containing cleaning liquid);
s9, cooling 1000L of refined extracting solution in the S8 in a crystallization tank for crystallization for 5.5 hours at the temperature of 12 ℃, stirring at the speed of 9 r/min, and filtering through a three-leg centrifuge after crystallization to obtain a filter cake;
s10, drying the filter cake obtained after filtration in the S9 for 8 hours at 82 ℃ under reduced pressure by using a rake dryer, crushing, packaging and warehousing to obtain 55.6kg of the finished product neohesperidin with the HPLC content of 95.7 percent and the yield of 5.56 percent.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. A method for preparing neohesperidin in physiological pomelo fruit drops by an alcohol/salt aqueous two-phase system is characterized by comprising the following steps: the method comprises the following steps:
s1: collecting the dried physiological dropped pomelo: the physiological fruit dropping of the pomelo or the artificial fruit dropping, and the sun drying or the oven drying are carried out, so that the raw materials are stably supplied during the industrial production;
s2: crushing and grinding: crushing a certain mass of dried pomelo physiological fallen fruits or artificially thinned fallen fruits in a hammer crusher, and grinding crushed coarse particles into powder by a wood flour machine to obtain pomelo dry powder;
s3: preparing and constructing a double water phase system: adding deionized water with the mass of 3-5 times of the dried pomelo powder into a liquid preparation tank, weighing food-grade NaH2PO4 inorganic salt with a certain mass, fully stirring and dissolving to prepare a NaH2PO4 solution with the mass fraction of 20%, and weighing 70% isopropanol with the same volume after fully dissolving to construct an isopropanol/NaH 2PO4 inorganic salt aqueous two-phase system with a certain mass and the pH = 4-5.5;
s4: and (3) hot dipping extraction: pumping the aqueous two-phase system in the step S3 into an extraction tank, adding the dried pomelo powder in the step S2, starting a machine to stir, controlling the rotating speed to be 50-80 r/min, carrying out hot reflux extraction for 2-3 h, and controlling the temperature to be 50-60 ℃;
s5: separating and phase-splitting of a liquid-solid three-phase disc separator: pumping the extracted material into a liquid-solid three-phase disc separator by a screw pump for separating and phase-splitting, controlling the feeding speed to be 2-5 cubic/h, and separating to obtain a solid phase, a light phase liquid and a heavy phase liquid;
s6: concentration: taking the light phase liquid to concentrate for 3-5 times at 65-75 ℃ in a single-effect falling-film evaporator to obtain a concentrated liquid with the baume degree of 3-8 DEG Be;
s7: water precipitation and crystallization and filtration: taking the concentrated solution, cooling to normal temperature, and mixing the concentrated solution according to the total weight of the concentrated solution of 1: 1-1.2 times of deionized water is added, and after uniform stirring, standing and crystallizing for 5 hours; filtering with a box-type filter press to obtain a neohesperidin crude product;
s8: and (3) ultrafiltration membrane assisted hot water recrystallization purification: putting all the neohesperidin crude products in S7 into a liquid preparation tank, adding 8-10 times of deionized water, heating to 80-85 ℃, stirring for 1-2 hours to fully dissolve the neohesperidin crude products, filtering to remove insoluble suspended matters by using a hollow fiber membrane at a pressure of 1.2-1.5 bar and a filtering speed of 500-600L/h to obtain clear filtrate, and performing ultrafiltration on the clear filtrate by using a GE4040 type 3500 Dalton ultrafiltration membrane at a pressure of 20-25 bar and a filtering speed of 500-600L/h to obtain refined extract;
s9: cooling and crystallizing: cooling and crystallizing the refined extract in the S8 in a crystallization tank for 5-8 h at 10-15 ℃, stirring at 5-10 r/min, and filtering by a three-legged centrifuge after crystallization to obtain a filter cake;
s10, drying and packaging: and (5) drying the filtered filter cake for 5-8 h at 80-85 ℃ through a rake dryer under reduced pressure, determining that the drying end point is when the detected moisture is less than 5%, packaging and warehousing to obtain a finished product of neohesperidin, wherein the HPLC content is more than or equal to 95%.
2. The method for preparing neohesperidin from physiological pomelo fruit drops by using the alcohol/salt aqueous two-phase system according to claim 1, which is characterized by comprising the following steps of: the aqueous two-phase system in the step S3 is isopropanol/NaH 2 PO 4 Inorganic salt system, naH 2 PO 4 The mass fraction of the solution is 20%, and 70% isopropanol has the same volume.
3. The method for preparing neohesperidin from physiological pomelo fruit drops by using the alcohol/salt aqueous two-phase system according to claim 1, which is characterized by comprising the following steps of: said NaH in step S3 2 PO 4 The inorganic salt is in a food grade,the execution standard is GB 25564-2010.
4. The method for preparing neohesperidin from physiological pomelo fruit drops by using the alcohol/salt aqueous two-phase system according to claim 1, which is characterized by comprising the following steps of: and the extraction tank in the step S4 is a dynamic extraction tank, and powder impregnation extraction is adopted.
5. The method for preparing neohesperidin from physiological pomelo fruit drops by using the alcohol/salt aqueous two-phase system according to claim 1, which is characterized by comprising the following steps of: the liquid-solid three-phase disc separator in the step S5 is an SDH200 type disc separator.
6. The method for preparing neohesperidin from physiological pomelo fruit drops by using the alcohol/salt aqueous two-phase system according to claim 1, which is characterized by comprising the following steps of: the hollow fiber membrane in the step S8 is a GE4040 type microfiltration membrane, and the filtration precision is 50 nanometers.
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| CN111662344B (en) * | 2020-06-29 | 2022-10-14 | 四川大学 | Method for recovering rebaudioside A from primary crystallization mother liquor of stevioside |
| CN111777653B (en) * | 2020-08-21 | 2023-07-21 | 江西海富生物工程有限公司 | Preparation method of pure natural high-content neohesperidin |
| CN112079884B (en) * | 2020-09-03 | 2023-06-02 | 江西海富生物工程有限公司 | Preparation method of natural neohesperidin |
| CN112125936A (en) * | 2020-09-09 | 2020-12-25 | 江西海富生物工程有限公司 | Method for extracting neohesperidin from fresh bitter orange fruits |
| CN112142807A (en) * | 2020-09-09 | 2020-12-29 | 江西海富生物工程有限公司 | Method for extracting neohesperidin from young fruits of lime |
| CN112047846B (en) * | 2020-10-13 | 2021-09-28 | 四川大学 | Method for extracting synephrine, naringin and neohesperidin from immature bitter oranges by using ultrasonic-assisted aqueous two-phase system |
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