Preparation method of neohesperidin without heavy metals
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A new hesperidin and heavy metal removal technology, which is applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., to achieve the effects of ensuring balance, reducing the effect of impurity removal, and improving product quality
Active Publication Date: 2020-09-18
JIANGXI HAIFU BIOENG
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[0020] The technical problem to be solved by the present invention is to overcome the existing traditional and old technology, start with the extraction, flocculation, separation, heavy metal removal and crystallization of raw materials, and innovatively adopt the low-temperature alcohol solution containing basic salt to remove impurities. , acid chitosan flocculation and ion exchange resin to remove impurities such as heavy metals, low-temperature alkoxide solution coarse crystallization and acetic acid recrystallization to extract, separate, purify and remove heavy metals to obtain pure natural neohesperidin products with high purity and no heavy metals , the preparation method is simple in process, strong in operability, and low in equipment requirements, and is a method that can realize large-scale production of heavy metal-removing neohesperidin
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preparation example 1
[0087] Preparation of modified chitosan: the modification method is the chloroacetic acid method. Specifically, after soaking and swelling 10g chitosan in 10L deionized water, add 50ml, 36% hydrochloric acid to fully dissolve it, and then add 10g sodium hydroxide and 40g of chloroacetic acid at a temperature of 40°C for 1 hour to carboxymethylate chitosan, and finally obtain it after separation and purification by ethanol precipitation.
Embodiment 1
[0089] 1. Impurity removal: After 50kg of citrus aurantium is broken, add 500kg in three times, pH is 4.5 (hydrochloric acid), basic zinc chloride concentration is 0.9%, ethanol volume fraction is the aqueous solution of 5% 4 ℃, each time Leakage and reflux for 4 hours, after bag centrifugation, collect and remove impurities;
[0090] 2. Extraction: Add 500kg of hot water at 90°C to the obtained residue for three times, stirring and extracting for 3 hours each time, centrifuging with cloth bag while it is hot, and collecting 363.2kg of extracting filtrate;
[0091] 3. Flocculation: Dissolve 2.5kg of the modified chitosan prepared in Preparation Example 1 in 10L of 1% acetic acid solution, then pour it all into the filtrate. A ceramic membrane with a molecular weight cut-off of 4000Da obtained a permeate of 335.6kg with a sugar content of 2.3brix;
[0092] 4. Chromatography: Put the permeate on the cation exchange chromatography column, the resin type is D113, the column volum...
Embodiment 2
[0099] Other operations and conditions are the same as in Example 1, except that in step 1, the basic salt is basic aluminum sulfate with a concentration of 1.5 wt%. Finally, the product neohesperidin is obtained. Through detection and calculation, it is obtained that the purity of the neohesperidin product is 99.3%, and the total yield is 92.1%; heavy metals in the product are not detected.
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Abstract
The invention provides a preparation method of neohesperidin without heavy metals. The preparation method comprises the following steps: (1) impurity removal: crushing raw materials, removing impurities by using a cold aqueous solution containing basic salt and alcohol, filtering and collecting impurity-removed residues; (2) extraction; (3) flocculation: adding a flocculating agent into permeate,flocculating under an acidic condition, then performing solid-liquid separation, and collecting the permeate overnight; (4) chromatography: enabling the obtained permeate to pass through a cation exchange column, and collecting effluent; (5) coarse crystallization; (6) recrystallization: dissolving the obtained coarse crystals, and then recrystallizing; (7) nanofiltration; and (8) drying and crushing. According to the method provided by the invention, extraction separation, purification and heavy metal removal are performed by adopting the processes of removing impurities by using a low-temperature basic salt alcohol solution, flocculating by using acidic chitosan, removing impurities such as heavy metals by using ion exchange resin, performing coarse crystallization by using a low-temperature alkoxide solution, recrystallizing by using acetic acid and the like, so that a pure natural neohesperidin product with high purity and no heavy metals is obtained, the purity of the neohesperidin is 98 percent or above, and the yield is 90 percent or above.
Description
technical field [0001] The invention relates to the field of natural product extraction, in particular to a method for preparing heavy metal-removing neohesperidin. Background technique [0002] Neohesperidin is a dihydroflavonoid compound composed of 3,5,7-trihydroxy-4-methoxyflavone as a glycoside ligand and rhamnosyl β-1,2 as a glycoside ligand. - Glycosides consisting of two units of glucose. Neohesperidin is weakly acidic, white needle-like crystals, easily soluble in hot water, soluble in hot ethanol, and insoluble in ether. Carbon dioxide does not precipitate in alkaline solution. Under strong acidic conditions, it is prone to hydrolysis to produce glucose, tangeretin and rhamnose. Neohesperidin has activities such as scavenging free radicals, promoting gastric motility, lowering blood lipids, anti-atherosclerosis, protecting the nervous system, anti-allergic, and anti-cancer, and has a wide range of uses in medicine; at the same time, neohesperidin is also a An i...
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