CN103521173A - Adsorbing agent capable of adsorbing zearalenone in feed and preparation method thereof - Google Patents
Adsorbing agent capable of adsorbing zearalenone in feed and preparation method thereof Download PDFInfo
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- CN103521173A CN103521173A CN201310491486.9A CN201310491486A CN103521173A CN 103521173 A CN103521173 A CN 103521173A CN 201310491486 A CN201310491486 A CN 201310491486A CN 103521173 A CN103521173 A CN 103521173A
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Abstract
The invention provides an adsorbing agent capable of adsorbing zearalenone in a feed and a preparation method thereof. The adsorbing agent uses modified halloysite to adsorb the zearalenone in mildewed grains pointedly and is an aluminosilicate adsorbing agent for adsorbing the zearalenone in the mildewed feed of livestock. The adsorbing agent takes the halloysite as a material. The preparation method comprises the following steps: soaking by a certain proportion of a surfactant antibacterial material (octadecyl dimethyl benzyl ammonium chloride), stirring, washing with water, filtering, drying, and grinding into powder, thus obtaining the adsorbing agent. For the treated halloysite, the dispersity is increased, the surface activity is improved and the adsorbing capability is enhanced.
Description
Technical field
This invention relates to feed safety and removing toxic substances field, be specifically related to a kind of can adsorption feed in the adsorbent and preparation method thereof of zearalenone.
Background technology
Zearalenone (Zearalenone, ZEN), is a kind of on-steroidal oestrogen-like hormone toxin that sickle-like bacteria produces, and is extensively present in the middle of cereal and feed.Zearalenone all may produce in results, transportation and storage process, because of its deposition effect relatively stable, can be along with food chain enters human body, the production of livestock and poultry and people's health has been produced to serious impact, cause huge economic loss, become agricultural and the very important problem of animal husbandry.There are some researches show zearalenone to all toxic effect, particularly female organ and the developments of fetus of immune system, internal system and reproductive system.The agenda of herding worker and medical worker has been put in the toxic action of how controlling and reducing zearalenone.In view of the consideration of economy and convenience, the method that reduces toxin harm mainly concentrates on develops nontoxic adsorbent.
At present, the main using microbe method of place to go ZEN and physical method adsorb or degrade.Microbial process is mainly that using fungus cell membrane and compound thereof carry out biodegradation to mycotoxin, and not only production process is loaded down with trivial details, and condition is wayward, and cost is higher, and product is stable not, and microorganism itself cannot be determined and be got rid of the effect of animal.And physical method is comparatively safe: adsorbent wide material sources, stable in properties, with low cost, easy and simple to handle are the absorbing mycotoxin methods of generally approving and adopting at present.
Galapectite is a kind of of natural silicate clay mineral, i.e. halloysite, and natural galapectite mineral have the similar hollow tubular structure of CNT, high specific area, good chemistry and heat endurance, for its application provides wide prospect.The good characteristic of natural galapectite has caused the extensive concern of Chinese scholars and has conducted in-depth research, as realized target administration treatment etc. as catalyst carrier or by useful as drug carrier after surface treatment.Montmorillonite is different as basic adsorbent with medical stone from take at present, and the security of galapectite is higher, in physianthropy field, applies; Its hollow tubular structural stability is good, has increased adsorption area simultaneously.Although natural minerals has lot of advantages, yet it is directly utilized, adsorption capacity does not often reach requirement, and therefore, much research has carried out take improving to natural minerals the modification that adsorption capacity is object.To sum up show: by galapectite surface, carry out chemical treatment or modification, can further improve its performance, bring into play the effect of its good absorbing mycotoxin.
Summary of the invention
Based on above weak point, the present invention disclose a kind of can adsorption feed in the adsorbent and preparation method thereof of zearalenone.Aim to provide a kind of for adsorbing the go mouldy Aluminosilicates adsorbent of zearalenone of feed of livestock and poultry.
Object of the present invention is achieved through the following technical solutions:
A preparation method for the adsorbent of zearalenone in can adsorption feed is as follows:
(1) take the natural galapectite of 100g, be crushed to 100 orders;
(2) press the natural galapectite of 5mg stearyl dimethyl benzyl ammonium chloride: 100g, add the ratio of 1000mL distilled water to mix;
(3) 50 ℃ of waters bath with thermostatic control, with the speed concussion of 5000rpm, react 10 minutes;
(4) after reaction completes, the centrifugal suspension that inclines, by the distilled water immersion of solid-to-liquid ratio mg:mL=20:100,50 ℃ of waters bath with thermostatic control are vibrated 15 minutes, and this process repeats 5 times;
(5) filter to be placed in 80 ℃ of baking ovens and dry 6 hours, be crushed to 100 order particles after cooling, standby.
The present invention also has following technical characterictic:
1, by as above prepared by method a kind of can adsorption feed in the adsorbent of zearalenone;
2, by as above prepared by method a kind of can adsorption feed in the adsorbent of zearalenone, it presses mass fraction 1% and adds in feed.
Galapectite decentralization after method of the present invention is processed increases, and surface-active increases, and adsorption capacity strengthens, and has reduced the toxic action that zearalenone produces body.
Accompanying drawing explanation
Galapectite figure under Fig. 1 ESEM;
Modification galapectite figure under Fig. 2 ESEM;
Galapectite figure under Fig. 3 transmission electron microscope;
Modification galapectite figure under Fig. 4 transmission electron microscope.
The specific embodiment
The applied reagent of the present invention can be applied arbitrary money commercially available prod, and zearalenone (ZEN) standard items are purchased from ENZO company (article No. is ALX-630-105-M050), high performance liquid chromatograph (HPLC) model is that Waters LC600, methyl alcohol and acetonitrile are all purchased from Sigma company.The compound method of buffer solution used is as follows:
1,5.0N hydrochloric acid: measure the concentrated hydrochloric acid of 214.8mL36%, join in 785.2mL distilled water.
2,0.2M NaOH: take 8.5g NaOH, join in 1000mL distilled water.
3,0.2M hydrochloric acid: measure the concentrated hydrochloric acid of 17mL36%, join in 983mL distilled water.
4, SGF: 8.3g stomach cardia peptone, 3.5gD-glucose, 2.05g sodium chloride, 0.6g potassium hydrogen phosphate, 0.11g calcium chloride, 0.37g potassium chloride, 0.1g lysozyme and 13.3mg pepsin adjust pH to be settled to 1000mL after 1.5 with the hydrochloric acid of 5.0N.
5, simulated intestinal fluid: 6.8g potassium dihydrogen phosphate is dissolved in 250mL distilled water, mixes with NaOH, 500mL water and the 10.0g pancreatin of 77mL0.2M.Take 0.2M NaOH or 0.2M hydrochloric acid, to adjust mixed solution pH value be 6.8 rear constant volume 1000mL.
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, and advantage and disadvantage of the present invention will be more clear along with description.But these embodiment are only exemplary, scope of the present invention are not formed to any restriction.
Embodiment 1
Natural galapectite modified test
1, modification galapectite preparation method
Take the natural galapectite of 100g, be crushed to 100 orders; 5mg stearyl dimethyl benzyl ammonium chloride and the natural galapectite of 100g are joined in 1000mL distilled water; 50 ℃ of waters bath with thermostatic control, with the speed concussion of 5000rpm, react 10 minutes; After reaction completes, the centrifugal suspension that inclines, by the distilled water immersion of solid-to-liquid ratio mg:mL=20:100,50 ℃ of waters bath with thermostatic control are vibrated 15 minutes, and this process repeats 5 times; Filter to be placed in 80 ℃ of baking ovens and dry 6 hours, be crushed to 100 order particles after cooling, standby.
2, the galapectite after electron microscopic observation modification
By ESEM picture, can find out (as shown in Figure 1): the galapectite after surfactant modification, by crumb structure closely originally, become the state of tiling, its uniformity and decentralization obviously increase, be easy to mix in feed, galapectite after modification and the contact area of toxin increase, and the new features of modification galapectite are more conducive to adsorb ZEN.
By transmission electron microscope, can find out clearly the nano tubular structure (as shown in Figure 2) of galapectite: compare with the galapectite that does not carry out modification, galapectite after modification, its tubulose internal diameter nearly doubles, and (mean inside diameter is increased to 20.12nm by 11.35nm, difference reaches the level of signifiance), outer surface becomes coarse simultaneously, further increase the contact area of itself and toxin, strengthened the absorption property of galapectite.
Embodiment 2:
The impact of modification galapectite addition on ZEN standard items adsorption rate
According to chyme time of staying in animal intestines and stomach, be determined at respectively the adsorption rate of modification galapectite addition to ZEN standard items under simulated animal stomach, intestinal environment, to determine the optimum addition of modification galapectite.
1, the impact of modification galapectite addition on ZEN adsorption rate in SGF
In sterilizing centrifuge tube, add 10mL SGF, 0.5mgZEN standard items, add respectively 4mg, 7mg, 10mg, 13mg, 16mg modification galapectite and 10mg galapectite, every group of 2 repetitions, 37 ℃ of concussion 4h, it is centrifugal that cultivation finishes rear 4000r/min, and HPLC method is measured ZEN content in supernatant, and calculate the adsorption efficiency of modification galapectite to ZEN, result is as shown in table 1.
The impact of modification galapectite addition on ZEN standard items adsorption rate under the in-vitro simulated gastric environment of table 1
2, the impact of modification galapectite addition on ZEN adsorption rate in simulated intestinal fluid
In sterilizing centrifuge tube, add 10mL simulated intestinal fluid, 0.5mgZEN standard items, add respectively 4mg, 7mg, 10mg, 13mg, 16mg modification galapectite and 10mg galapectite, every group of 2 repetitions, 37 ℃ of concussion 8h, it is centrifugal that cultivation finishes rear 4000r/min, and HPLC method is measured ZEN content in supernatant, and calculate the adsorption efficiency of modification galapectite to ZEN, experimental result is in Table 2.
The impact of modification galapectite addition on ZEN standard items adsorption rate under the in-vitro simulated intestines environment of table 2
By table 1, table 2 can find out, the galapectite adsorption rate after modification obviously improves, and approaches the adsorption effect of montmorillonite.When modification galapectite addition is during lower than 1g/L, along with the increase of addition, ZEN degradation rate improves constantly; When addition is during higher than 1g/L, along with the increase of addition, ZEN degradation rate tends towards stability, so the suitableeest addition of modification galapectite is 1g/L.
Embodiment 3:
The impact of the adsorption time of modification galapectite on ZEN standard items adsorption rate
Under simulated animal stomach, intestinal environment, the modification galapectite of measuring respectively the suitableeest addition is the adsorption rate to ZEN at different adsorption times, to determine the optimal adsorption time of modification galapectite.
1, modification galapectite determining ZEN adsorption time in SGF
In sterilizing centrifuge tube, add 10mL SGF, 0.5mgZEN standard items, add 10mg modification galapectite, every group of 2 repetitions, concussion at 37 ℃, when 20min, 40min, 60min, 90min and 120min, by HPLC method, measure ZEN content in supernatant respectively, and calculate the adsorption efficiency of modification galapectite to ZEN, experimental result is in Table 3.
The impact of modification galapectite adsorption time on ZEN standard items adsorption rate under the in-vitro simulated gastric environment of table 3
2, modification galapectite determining ZEN adsorption time in simulated intestinal fluid
In sterilizing centrifuge tube, add 10mL simulated intestinal fluid, 0.5mgZEN standard items, add 10mg modification galapectite, every group of 2 repetitions, concussion at 37 ℃, when 30min, 60min, 90min, 120min and 240min, by HPLC method, measure ZEN content in supernatant respectively, and calculate the adsorption efficiency of modification galapectite to ZEN, experimental result is in Table 4.
The impact of modification galapectite adsorption time on ZEN standard items adsorption rate under the in-vitro simulated intestines environment of table 4
By table 3, table 4 can find out, the galapectite after modification at different adsorption times to the adsorption rate of ZEN all higher than unmodified galapectite.When modification galapectite addition is 10mg, along with the prolongation of degradation time, the degradation rate of ZEN improves constantly; Simulate in vitro in gastric environment, when degradation time >=90min, the degradation rate of ZEN tends towards stability; Simulate in vitro in intestines environment, during degradation time >=2h, ZEN degradation rate tends towards stability.
In sum, modification galapectite is significantly improved than unmodified galapectite adsorption effect, approaches montmorillonite.The optimum condition of modification galapectite degraded ZEN standard items is: bacterium powder addition 1g/L, 37 ℃, pH1.5, degraded 1.5h; 37 ℃, pH6.8, degraded 2.0h, now the highest to the total degradation rate of ZEN standard items, reach 81.4%.
Embodiment 4:
The suction-operated of modification galapectite to ZEN in mouldy corn
1, the total quantitative determination of ZEN in mouldy corn
After mouldy crush maize, cross 20 mesh sieves, according to the requirement of the assay method of zearalenone in State Standard of the People's Republic of China-cereal (GB/T5009.209-2008), the content of measuring ZEN is: 2765.34ppb.
2, the impact of modification galapectite addition on ZEN adsorption rate in mouldy corn
According to chyme time of staying in animal intestines and stomach, be determined at respectively under simulated animal stomach, intestinal environment, the impact of modification galapectite addition on the adsorption rate of ZEN in mouldy corn, determines the optimum addition of modification galapectite.
(1) impact of modification galapectite addition on ZEN adsorption rate in SGF
In sterilizing centrifuge tube, add 10mL SGF, mouldy corn 5g, add respectively 4mg, 7mg, 10mg, 13mg, 16mg modification galapectite and 10mg galapectite, every group of 2 repetitions, 37 ℃ of concussion 4h, it is centrifugal that cultivation finishes rear 4000r/min, and HPLC method is measured ZEN content in supernatant, and calculate the adsorption efficiency of modification galapectite to ZEN, experimental result is in Table 5.
The impact of modification galapectite addition on ZEN adsorption rate under the in-vitro simulated gastric environment of table 5
(2) impact of modification galapectite addition on ZEN adsorption rate in simulated intestinal fluid
In sterilizing centrifuge tube, add 10mL simulated intestinal fluid, mouldy corn 5g, add respectively 4mg, 7mg, 10mg, 13mg, 16mg modification galapectite and 10mg galapectite, every group of 2 repetitions, 37 ℃ of concussion 8h, it is centrifugal that cultivation finishes rear 4000r/min, and HPLC method is measured ZEN content in supernatant, and calculate the adsorption efficiency of modification galapectite to ZEN, experimental result is in Table 6.
The impact of modification galapectite addition on ZEN adsorption rate under the in-vitro simulated intestines environment of table 6
By table 5, table 6 can find out, the galapectite adsorption rate after modification obviously improves, and approaches the adsorption effect of montmorillonite.When modification galapectite addition is during lower than 1g/L, along with the increase of addition, ZEN degradation rate improves constantly; When addition is during higher than 1g/L, along with the increase of addition, ZEN degradation rate tends towards stability, so the suitableeest addition of modification galapectite is 1g/L.
The impact of the adsorption time of 3 modification galapectites on ZEN adsorption rate in mouldy corn
Under simulated animal stomach, intestinal environment, the modification galapectite of measuring respectively the suitableeest addition different adsorption times to mouldy corn in the adsorption rate of ZEN, to determine the optimal adsorption time of modification galapectite.
(1) modification galapectite determining ZEN adsorption time in mouldy corn in SGF
In sterilizing centrifuge tube, add 10mL SGF, mouldy corn 5g, add 10mg modification galapectite, every group of 2 repetitions, concussion at 37 ℃, when 20min, 40min, 60min, 90min and 120min, by HPLC method, measure ZEN content in supernatant respectively, and calculate the adsorption efficiency of modification galapectite to ZEN, experimental result is in Table 7.
The impact of modification galapectite adsorption time on ZEN adsorption rate under the in-vitro simulated gastric environment of table 7
(2) modification galapectite determining ZEN adsorption time in mouldy corn in simulated intestinal fluid
In sterilizing centrifuge tube, add 10mL simulated intestinal fluid, mouldy corn 5g, add 10mg modification galapectite, every group of 2 repetitions, concussion at 37 ℃, when 30min, 60min, 90min, 120min and 240min, by HPLC method, measure ZEN content in supernatant respectively, and calculate the adsorption efficiency of modification galapectite to ZEN, experimental result is in Table 8.
The impact of modification galapectite adsorption time on ZEN adsorption rate under the in-vitro simulated intestines environment of table 8
By table 7, table 8 can find out, the galapectite after modification at different adsorption times to the adsorption rate of ZEN all higher than unmodified galapectite.When modification galapectite addition is 10mg, along with the prolongation of degradation time, the degradation rate of ZEN improves constantly; Simulate in vitro in gastric environment, when degradation time >=90min, the degradation rate of ZEN tends towards stability; Simulate in vitro in intestines environment, during degradation time >=2h, ZEN degradation rate tends towards stability.
In sum, modification galapectite is significantly improved than unmodified galapectite adsorption effect, approaches montmorillonite.The modification galapectite optimum condition of ZEN in mouldy corn of degrading is: bacterium powder addition 1g/L, 37 ℃, pH1.5, degraded 1.5h; 37 ℃, pH6.8, degraded 2.0h, now the highest to the total degradation rate of ZEN in mouldy corn, reach 76.1%.
Embodiment 5:
The adsorption effect of modification galapectite to ZEN in rat body
Growing up, Sprague-Dawley rat (female mouse) is 1% modification galapectite adsorbent containing adding mass fraction in 0.5mg/kg zearalenone (ZEN) daily ration.Adsorption effect is as shown in table 9.Compare with control group, rat organ organizes ZEN residual quantity to decline, and growth performance improves, and has reduced the toxic action that ZEN produces body.
The adsorption effect of table 9 modification galapectite to ZEN in rat body
Claims (3)
1. in can adsorption feed, a preparation method for the adsorbent of zearalenone, is characterized in that, step is as follows:
(1) take the natural galapectite of 100g, be crushed to 100 orders;
(2) press the natural galapectite of 5mg stearyl dimethyl benzyl ammonium chloride: 100g, add the ratio of 1000mL distilled water to mix;
(3) 50 ℃ of waters bath with thermostatic control, with the speed concussion of 5000rpm, react 10 minutes;
(4) after reaction completes, the centrifugal suspension that inclines, by the distilled water immersion of solid-to-liquid ratio mg:mL=20:100,50 ℃ of waters bath with thermostatic control are vibrated 15 minutes, and this process repeats 5 times;
(5) filter to be placed in 80 ℃ of baking ovens and dry 6 hours, be crushed to 100 order particles after cooling, standby.
According to claim 1 a kind of can adsorption feed in the preparation method of adsorbent of zearalenone make a kind of can adsorption feed in the adsorbent of zearalenone.
According to claim 2 a kind of can adsorption feed in the adsorbent of zearalenone, it is characterized in that, it presses mass fraction 1% and adds in feed.
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| CN107159140A (en) * | 2017-06-05 | 2017-09-15 | 中国科学院兰州化学物理研究所盱眙凹土应用技术研发中心 | The preparation method of organo-mineral complexing attapulgite mold toxin sorbent |
| CN107279688A (en) * | 2017-07-01 | 2017-10-24 | 河北工业大学 | A kind of complex mineral takes off mould dose and preparation method thereof |
| CN107744051A (en) * | 2017-11-23 | 2018-03-02 | 安徽金牧饲料有限公司 | A kind of odorless type cattle and sheep feed of natural high microsteping |
| CN107788207A (en) * | 2017-11-23 | 2018-03-13 | 安徽金牧饲料有限公司 | A kind of ecological fermentation feed |
| EP3315030A1 (en) * | 2016-10-27 | 2018-05-02 | CIECH R&D Sp. z o.o. | Halloysite for use as a feed additive and method to increase growth, viability and performance of poultry |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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