CN104045734B - A kind of process for preparing resins that there is efficient absorption to act on to patulin - Google Patents
A kind of process for preparing resins that there is efficient absorption to act on to patulin Download PDFInfo
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- CN104045734B CN104045734B CN201410321994.7A CN201410321994A CN104045734B CN 104045734 B CN104045734 B CN 104045734B CN 201410321994 A CN201410321994 A CN 201410321994A CN 104045734 B CN104045734 B CN 104045734B
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- patulin
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- resins
- absorption
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Abstract
The present invention relates to a kind of process for preparing resins that there is efficient absorption to act on to patulin.The present invention prepares polysaccharide resins using polysaccharide as raw material through processes such as absorption, scattered, emulsification, precrosslink, crosslinking, elution and modifications.Polysaccharide resins prepared by the present invention, with short production cycle, preparation technology is simple, product specification is homogeneous, it is with low cost the features such as, be suitable for industrial production.Polysaccharide resins product shows white or faint yellow prepared by the present invention, uniform particle diameter, quality is good, safety non-toxic, available for the absorption of patulin in the fields such as fruit juice, beverage, patulin excessive problem is efficiently solved, with good application prospect.
Description
Technical field
The present invention relates to a kind of process for preparing resins that there is efficient absorption to act on to patulin.Prepared with the present invention
Resin is high to patulin adsorption efficiency, and simple production process is with low cost, and uses safety.A kind of new exhibition can be used as
Penicillin sorbing material, is widely used in the fields such as fruit juice, beverage.
Background technology
Patulin is a kind of mycotoxin, to zooblast and tissue with very strong toxicity, easily pollute fruit and
Its product, and stabilization time is most long in apple base beverage.The World Health Organization has to the threshold limit values of patulin in food
Strict regulation（The μ g/L of ＜ 50）, and have the trend constantly reduced.Nowadays people gradually increase to the consumption figure of fruit and fruit juice
Greatly, and China is the first big country of apple and its inspissated juice production again, concentrated apple juice export ratio is up to more than 90%, and it is led
It is the U.S., Europe and Japan to want market.Patulin pollution turns into puzzlement fruit juice, a great problem of beverage production industry.
The technology for eliminating of patulin in fruit juice, beverage is rarely reported at present.Turn into a kind of effective using resin adsorption
The method for reducing patulin, the material source for preparing resin is extensive, including agarose, starch, cellulose, chitosan or shell are few
Sugar etc., this method has the low advantage of easy to operate, use cost.
Polysaccharide resins have the characteristics of adsorption range is extensive, and it need to be carried out chemical modification to strengthen it to patulin
Selectivity, so as to reduce its influence to beneficiating ingredient in fruit juice, beverage.
The content of the invention
The present invention is to provide a kind of resin for efficient absorption patulin, and its preparation method is：Polysaccharide powder is molten
In reagent 1. solution, crosslinking is carried out using crosslinking agent and prepares polysaccharide resins, first with petroleum ether, acetone and ethanol cyclic washing,
Afterwards with reagent 2. solution graft copolymerization modification of polysaccharides resin, dried at 20 ~ 60 DEG C, obtain the resin of efficient absorption patulin.
Reagent described in above-mentioned technological process 1. and 2., respectively acetic acid or hydrochloric acid and thiocarbamide or thiosemicarbazides or two sulphur
Change carbon solution；Crosslinking agent is formaldehyde and glutaraldehyde, or formaldehyde and epoxychloropropane, or formaldehyde and ethylene glycol diglycidylether；
Polysaccharide is any one of agarose, starch, cellulose, chitosan or chitosan oligosaccharide.
This product is a kind of a diameter of 20 ~ 500 μm spherical small porous particle, white or yellow.The product is insoluble in conventional
Organic solvent, such as acetone, ethyl acetate, chloroform, ether.The product uses pH scopes 2.0 ~ 12.0, temperature in use scope 4
~40 ℃；This product has efficient absorption effect to patulin, can be applied in terms of fruit juice, beverage.
Embodiment：
2 ~ 20 g polysaccharide powders are dissolved in 1% ~ 5% acetic acid solution.Formaldehyde and penta is respectively adopted under the conditions of 20 ~ 80 DEG C
Dialdehyde or epoxychloropropane or ethylene glycol diglycidylether make precrosslinker and crosslinking agent prepares polysaccharide resins, after use oil
Ether, acetone and ethanol cyclic washing；By the resin and 0.1 ~ 2.0% thiocarbamide or thiosemicarbazides or carbon disulfide solution after washing
React 24 h.Reacted resin is washed to neutrality, the resin finished product of efficient absorption patulin is made in 20 ~ 60 DEG C of drying.
Example 1：10 g chitosans are taken to be dissolved in 24 h in 2% acetic acid solution.Formaldehyde is respectively adopted under the conditions of 40 DEG C and 60 DEG C
Chitosan resin is prepared as precrosslinker and crosslinking agent with glutaraldehyde, afterwards with petroleum ether, acetone and ethanol cyclic washing.It will wash
Chitosan resin and the h of 0.5% thiosemicarbazides solution reaction 24 after washing.Reacted resin is washed to neutrality, 20 ~ 60 DEG C of bakings
It is dry, the resin finished product of efficient absorption patulin is made.
Example 2：10 g agaroses are taken to be dissolved in 24 h in 2% hydrochloric acid solution.Formaldehyde is respectively adopted under the conditions of 40 DEG C and 60 DEG C
Agarose resin is prepared as precrosslinker and crosslinking agent with epoxychloropropane, afterwards with petroleum ether, acetone and ethanol cyclic washing.
Agarose resin after washing and 0.5% thiourea solution are reacted into 24 h.Reacted resin is washed to neutrality, 20 ~ 60 DEG C of bakings
It is dry, the resin finished product of efficient absorption patulin is made.
Example 3：10 g chitosan oligosaccharides are taken to be dissolved in 24 h in 2% acetic acid solution.Benzene first is respectively adopted under the conditions of 40 DEG C and 60 DEG C
Aldehyde and ethylene glycol diglycidylether prepare chitosan oligosaccharide resin as precrosslinker and crosslinking agent, afterwards with petroleum ether, acetone and second
Alcohol cyclic washing.By the chitosan oligosaccharide resin after washing respectively with 0.5% thiocarbamide and the h of thiosemicarbazides solution reaction 24.After reacting
Resin wash to neutrality, the resin finished product of efficient absorption patulin is made in 20 ~ 60 DEG C of drying.
Claims (2)
1. a kind of purposes for the resin that there is efficient absorption to act on to patulin, it is characterised in that：Applied in fruit juice, beverage
Patulin absorption；
The preparation method of the resin is as follows：
(1) 2~20g of polysaccharide powder is dissolved in 8~36h in 1%~5% acetic acid solution, is respectively adopted and pre-pays at 20~80 DEG C
Connection agent and crosslinking agent prepare polysaccharide resins, and petroleum ether, acetone and ethanol cyclic washing are used afterwards；
(2) modifying agent is dissolved in solvent, fully dissolving, adds 5~10g of polysaccharide resins, water-bath vibration 12-48h；
(3) by above-mentioned modification of polysaccharides resin suction filtration, clean to neutrality, be put into 0.1~1mol/L sodium hydroxide solutions, water-bath is shaken
6~24h is swung, obtained modification of polysaccharides resin is washed to neutrality, is dried at 20~60 DEG C, resin finished product is made；
Polysaccharide is one kind in chitosan, agarose, starch, cellulose, cyclodextrin and chitosan oligosaccharide in described (1)；
Precrosslinker is one kind in formaldehyde, benzaldehyde in described (1)；Crosslinking agent is glutaraldehyde, epoxychloropropane and second two
One kind in alcohol diglycidyl ether；
The modifying agent used in described (2) is 1~3 kind in thiocarbamide, thiosemicarbazides and carbon disulfide.
2. there is the purposes of the resin of efficient absorption effect according to claim 1 to patulin, it is characterised in that：Described
(3) water-bath vibration is vibrated for water-bath at room temperature in.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410321994.7A CN104045734B (en) | 2014-07-08 | 2014-07-08 | A kind of process for preparing resins that there is efficient absorption to act on to patulin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410321994.7A CN104045734B (en) | 2014-07-08 | 2014-07-08 | A kind of process for preparing resins that there is efficient absorption to act on to patulin |
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| Publication Number | Publication Date |
|---|---|
| CN104045734A CN104045734A (en) | 2014-09-17 |
| CN104045734B true CN104045734B (en) | 2017-11-07 |
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| CN201410321994.7A Active CN104045734B (en) | 2014-07-08 | 2014-07-08 | A kind of process for preparing resins that there is efficient absorption to act on to patulin |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105268410B (en) * | 2015-11-26 | 2017-12-08 | 内蒙古科技大学 | A kind of preparation method and application method of antibiotic adsorbed film |
| CN108295818A (en) * | 2018-01-19 | 2018-07-20 | 浙江理工大学 | A method of preparing heavy metal ion adsorbing material using thiosemicarbazides modification bamboo pulp fiber element |
| CN110038524B (en) * | 2019-03-20 | 2021-11-12 | 江西师范大学 | Preparation method of affinity chromatography medium for separating and purifying chitosanase |
| CN114887592A (en) * | 2022-04-22 | 2022-08-12 | 江苏第二师范学院 | Preparation and application of thiosemicarbazone silicon dioxide microsphere material |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000264902A (en) * | 1999-03-15 | 2000-09-26 | Univ Miyazaki | Thiourea derivative of chitosan |
| CN1269535C (en) * | 2003-07-15 | 2006-08-16 | 南开大学 | Spherical amino acid adsorbent and its preparation method |
| CN103772573B (en) * | 2014-02-24 | 2016-08-17 | 艾美科健（中国）生物医药有限公司 | A kind of superhigh cross-linking macroporous adsorbent resin being applicable to clavacin removing |
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