CN109351344A - Ochracin adsorbent material, preparation method and applications in a kind of corn - Google Patents
Ochracin adsorbent material, preparation method and applications in a kind of corn Download PDFInfo
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- CN109351344A CN109351344A CN201811122677.7A CN201811122677A CN109351344A CN 109351344 A CN109351344 A CN 109351344A CN 201811122677 A CN201811122677 A CN 201811122677A CN 109351344 A CN109351344 A CN 109351344A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/261—Synthetic macromolecular compounds obtained by reactions only involving carbon to carbon unsaturated bonds
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/045—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium containing sulfur, e.g. sulfates, thiosulfates, gypsum
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/223—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention discloses ochracin adsorbent materials, preparation method and applications in a kind of corn, and the method is specifically: including obtaining calcination after tetrabutylammonium chloride, sodium sulphate and polyacrylamide-tetraethylenepentamine grafting chelating gel mixing；The temperature of the calcination is 120~150 DEG C；Tetrabutylammonium chloride, sodium sulphate and polyacrylamide-tetraethylenepentamine grafting chelating gel mass ratio are 1:7:2.The present invention prepares the adsorbent material method rapid and convenient, has very high targeting and arresting efficiency using special ion liquid, salt and grafting chelating gel, obtained adsorbent material when preparation, this method is to the permeability of ochracin in corn up to 99.2%.Wide with the range of linearity, detection limit is low, and relative standard deviation is smaller, is able to satisfy detection requirement of the country for ochracin in corn.
Description
Technical field
The invention belongs to Environmental Science and Engineering fields, and in particular to ochracin adsorbent material, preparation in a kind of corn
Method and its application.
Background technique
The toxigenic bacterium strain of ochracin has Aspergillus ochraceus and aspergillus sulphureus etc..The toxigenic bacterium strain of the dirty ochracin of ochracin
There are Aspergillus ochraceus and aspergillus sulphureus etc..The pollution range of ochracin is wider, can almost pollute corn, all cereal such as wheat,
And from the point of view of sample detection, there is pollution both at home and abroad.The acute toxicity of ochracin is stronger, and the LD50 of passing through mouth to duckling is only
0.5mg/kg weight is suitable with aflatoxins；LD50 of passing through mouth to rat is 20mg/kg weight.The cause of death of ochracin
It is the gangrenosum acne lesion of liver, kidney.It may separate out ochracin in the cereal for leading to Liver Cancer, the relationship with human liver cancer
Wait further to study.It is just in consideration of it, imperative to the improvement of ochracin capture material.
Cereals matrix is concentrated mainly on for the detection method of ochratoxin both at home and abroad at present, there is thin-layered chromatography
(TLC), enzyme-linked immunization (ELSA), immune affinity column-HPLC method and liquid chromatography tandem mass spectrometry etc..TLC method operation compared with
Complexity, organic solvent needed for extraction process is more, environment easy to pollute, has larger harm to human body, and sensitivity and special
Property is not high.Although ELSA method sensitivity is higher, false positive rate is also higher, thus is suitable only for quickly screening.Affine in immunity at present
Column-HPLC method is relatively common for detecting ochratoxin, and immune affinity column specificity is high, and HPLC standard measure is accurate, sensitivity
Height, but the disadvantage is that expensive, storage, traffic condition require height, and HPLC method is not final confirmation method.Liquid chromatogram-
Tandem mass spectrometry using more and more extensive, have in terms of anti-matrix interference ability, accurate qualitative and sensitivity relatively strong
Advantage, but still there are expensive, storage, the demanding problem of traffic condition.
There is black carbon (BC450) soil of addition to adsorb ochracin the adsorbent material of ochracin at present, operates
Simply, but there is a problem of low to the adsorption rate of ochracin, expensive.
For ionic liquid aqueous two-phase as a kind of novel green separation system occurred in recent years, itself has toxicity
It is small, the properties such as non-combustible, non-volatile, not oxidizable.Up to the present, about ionic liquid double-aqueous phase system as osmotic system
Data information also more lack, meanwhile, be also not seen reported, therefore the system ground about ionic liquid infiltration ochracin
Study carefully with far-reaching influence.
Summary of the invention
It is long for there are times of penetration in existing ochracin permeating method, equipment is expensive, complicated for operation, permeability is low
The disadvantages of, the purpose of the present invention is to provide ochracin adsorbent material, preparation method and applications in a kind of corn, the materials
Ochracin can be captured.
In order to realize that above-mentioned task, the present invention take following technical solution:
The preparation method of ochracin adsorbent material in a kind of corn, including by tetrabutylammonium chloride, sodium sulphate and poly- third
Calcination obtains after acrylamide-tetraethylenepentamine grafting chelating gel mixing；
The temperature of the calcination is 120~150 DEG C；
Tetrabutylammonium chloride, sodium sulphate and polyacrylamide-tetraethylenepentamine grafting chelating gel mass ratio are 1:7:
2。
Optionally, the time of the calcination is 2h, and powdery granule object is obtained after calcination；
Then powdery granule object is obtained to ochracin adsorbent material in the corn after vacuum dried.
Optionally, the vacuum drying temperature is 20~40 DEG C, and the vacuum drying time is 24~48h.
Optionally, the method is specifically: by sodium sulphate and tetrabutylammonium chloride, being mixed to get aqueous two-phase extraction body
System, then polyacrylamide-tetraethylenepentamine grafting chelating gel is added in two phase aqueous extraction system and obtains gel mixture, it coagulates
Glue mixture calcination obtains powdery granule object；
Then powdery granule object is obtained to ochracin adsorbent material in the corn after vacuum dried.
Ochracin adsorbent material in a kind of corn, the adsorbent material are prepared into using preparation method of the present invention
It arrives.
Application of the ochracin adsorbent material for ochracin absorption in corn in corn of the present invention.
Optionally, specifically using ochracin adsorbent material in corn of the invention for ochracin absorption in corn
Method includes: that mass ratio is corn: water: adsorbent material=4:8:1, stands 20min at 26 DEG C.
Compared with prior art, advantages of the present invention are as follows:
Adsorbent material preparation method rapid and convenient of the present invention, it is solidifying using special ion liquid, salt and grafting chelating when preparation
Glue, obtained regular hexagon active adsorbing material have very high targeting and arresting efficiency, and this method is to Aspergillus ochraceus in corn
The permeability of element has the range of linearity wide up to 99.2%, and detection limit is low, and relative standard deviation is smaller, and it is right to be both able to satisfy country
The detection requirement of ochracin in corn.Shorten ochracin disengaging time, while have it is easy to operate, without using large size
Instrument, the characteristics of reduction using traditional volatile organic solvent to avoid secondary pollution is brought.
Detailed description of the invention
The electromicroscopic photograph of ochracin adsorbent material in the corn that Fig. 1 is prepared for embodiment 1；
The electromicroscopic photograph of ochracin adsorbent material in the corn that Fig. 2 is prepared for embodiment 2；
The electromicroscopic photograph of ochracin adsorbent material in the corn that Fig. 3 is prepared for embodiment 3；
The present invention is further explained below in conjunction with the drawings and specific embodiments.
Specific embodiment
The preparation method rapid and convenient of ochracin adsorbent material in corn of the present invention uses special ion liquid when preparation
Body, salt and grafting chelating gel, obtained regular hexagon active adsorbing material have very high targeting and arresting efficiency, the party
Method up to 99.2%, has the range of linearity wide the permeability of ochracin in corn, and detection limit is low, relative standard deviation compared with
Small, specifically, tetrabutylammonium chloride: sodium sulphate: polyacrylamide-tetraethylenepentamine grafting chelating gel mass ratio is 1:7:
2。
Specific process for preparation can be with are as follows: the Cl and 63 part of quality of ionic liquid [TBA] for being 17% by 21 parts of mass fractions
The Na that score is 36%2SO4It is uniformly mixed, obtains aqueous two-phase osmotic system, adding 16 parts of mass fractions is 40%TEPA-
PAM-Gel obtains gelatinous mixture, and above-mentioned gelatinous mixture (is obtained powdered for calcination two hours at 120~150 DEG C
Particle), it is then stored at standing 24~48 hours in 20~40 DEG C of vacuum oven, the adsorbent material is made, is used for
The capture of ochracin in corn.
Tetrabutylammonium chloride: ([TBA] Cl), upper marine origin victory Chemical Co., Ltd.；
Polyacrylamide-tetraethylenepentamine grafting chelating gel (TEPA-PAM-Gel): with polyacrylamide gel (PAM-
Gel, Gongyi City source Yu Runhai water-purifying material Co., Ltd) it is skeleton, with tetraethylenepentamine (Jinan century limited public affairs of sensible chemical industry
Department) it is that grafting chelating agent reacts in formaldehyde presence according to Mannich, chelation group is made and is grafted gel；
The specific catching method of capture for the ochracin in corn is corn: water: adsorbent material=4:8:
1 mass ratio stands 20min at 26 DEG C, captures the ochracin in corn, takes out corn later, cleaned with clear water.Record
The permeability of capture front and back object is shown in Table one.
In order to realize the capture rate for improving ochracin in corn, it is more excellent to obtain that the present invention devises a series of experiments
Technological parameter:
Embodiment 1:
The Na for being 36% by Cl and 63 part of mass fraction of ionic liquid [TBA] that 21 parts of mass fractions are 17%2SO4Mixing
Uniformly, aqueous two-phase osmotic system is obtained, adding 16 parts of mass fractions is that 40%TEPA-PAM-Gel obtains gelatinous mixture,
Above-mentioned gelatinous mixture is obtained into powdery granule in calcination two hours at 150 DEG C, is then stored at 40 DEG C of vacuum
48 hours are stood in drying box, the adsorbent material is made.
Corn: water: adsorbent material=4:8:1 mass ratio stands 20min at 26 DEG C, captures the Aspergillus ochraceus in corn
Element takes out corn later, is cleaned with clear water.The permeability of record capture front and back object is shown in Table one.
Embodiment 2:
The preparation method of the present embodiment is same as Example 1, distinguishes the ionic liquid type being only that in preparation process not
Together, ionic liquid is changed to [CF3SO3] (trifluoromethayl sulfonic acid) in the present embodiment, remaining condition is constant, record capture front and back mesh
The permeability of mark object is shown in Table one.
Embodiment 3:
The preparation method of the present embodiment is same as Example 1, distinguishes the ionic liquid type being only that in preparation process not
Together, ionic liquid is changed to [bmim] Cl (chlorobutanol methylimidazole) in the present embodiment, remaining condition is constant, before record capture
The permeability of object is shown in Table one afterwards.
The ingredient that adsorbent material intermediate ion liquid is changed it can be seen from above-described embodiment and table one, for separating jade
The permeability of ochracin in rice is respectively 99.2%, 74.3%, 59.3%, and the separating effect to object gas is [TBA]
Cl > [CF3SO3] > [bmim] C, so the permeability of ochracin when using [TBA] Cl as ionic liquid in corn is most
Greatly, osmotic effect is best.
When adsorbent material intermediate ion liquid is [TBA] Cl it can be seen from Fig. 1,2 and 3, the knot of regular hexagon can be formed
Structure, and change ionic liquid type, structure changes, and the capture rate of original active adsorbing material reduces.
Embodiment 4:
The preparation method of the present embodiment is same as Example 1, distinguishes the condition difference being only that in preparation process, this implementation
Salt in example is changed to Na2CO3, remaining condition is constant, and the permeability of record capture front and back object is shown in Table one.
Embodiment 5:
The preparation method of the present embodiment is same as Example 1, distinguishes the condition difference being only that in preparation process, this implementation
Salt in example is changed to MgSO4, remaining condition is constant, and the permeability of record capture front and back object ochracin is shown in Table one.
The ingredient that salt is changed it can be seen from above-described embodiment and table one, for the ochracin in separating corn
Permeability is respectively 99.2%, 80.6%, 77.4%, and the separating effect to object gas is Na2SO4 > Na2CO3 > MgSO4, institute
The permeability of ochracin when using Na2SO4 as salt in corn is maximum, and osmotic effect is best.
Embodiment 6:
The preparation method of the present embodiment is same as Example 1, distinguishes the condition difference being only that in preparation process, this implementation
The mass fraction of ionic liquid in example is changed to 10%, remaining condition is constant, the infiltration of record capture front and back object ochracin
Saturating rate is shown in Table one.
Embodiment 7:
The preparation method of the present embodiment is same as Example 1, distinguishes the condition difference being only that in preparation process, this implementation
The mass fraction of ionic liquid in example is changed to 24%, remaining condition is constant, and the permeability of record capture front and back object is shown in Table
One.
The mass fraction for changing ionic liquid it can be seen from above-described embodiment and table one, for reddish brown in separating corn
The permeability of aspergillin is respectively 99.2%, 80.0%, 79.4%, thus the use of mass fraction is 17% ionic liquid when it is beautiful
The permeability of ochracin in rice is maximum, and osmotic effect is best.
Embodiment 8:
The preparation method of the present embodiment is same as Example 1, distinguishes the condition difference being only that in preparation process, this implementation
The type of gel in example is changed to rice bran wax, remaining condition is constant, and the permeability of record capture front and back object is shown in Table one.
Embodiment 9:
The preparation method of the present embodiment is same as Example 1, distinguishes the condition difference being only that in preparation process, this implementation
The type of gel in example is changed to oryzanol, remaining condition is constant, and the permeability of record capture front and back object is shown in Table one.
The type for changing three kinds of gels it can be seen from above-described embodiment and table one, for the Aspergillus ochraceus in separating corn
The permeability of element is respectively 99.2%, 63.0%, 84.1%, so using the ochracin in corn when TEPA-PAM-Gel
Permeability is maximum, and osmotic effect is best.
Embodiment 10:
The preparation method of the present embodiment is same as Example 1, and difference is only that preparation process conditional is different, the present embodiment
In the mass fraction of gel be changed to 30%, remaining condition is constant, and the permeability of record capture front and back object ochracin is shown in
Table one.
Embodiment 11:
The preparation method of the present embodiment is same as Example 1, distinguishes the condition difference being only that in preparation process, this implementation
The mass fraction of gel in example is changed to 50%, remaining condition is constant, the permeability of record capture front and back object ochracin
It is shown in Table one.
The mass fraction for changing gel it can be seen from above-described embodiment and table one, for the Aspergillus ochraceus in separating corn
The permeability of element is respectively 99.2%, 77.4%, 89.5%, so accounting for total quality of materials using addition is 40%TEPA-PAM-
The permeability of ochracin when Gel in corn is maximum, and osmotic effect is best.
Embodiment 12:
The preparation method of the present embodiment is same as Example 1, and difference is only that the object of adsorbent material effect is different, this
Object in embodiment is changed to aflatoxins, remaining condition is constant, and the permeability of record capture front and back object is shown in Table one.
Embodiment 13:
The preparation method of the present embodiment is same as Example 1, and difference is only that the object of adsorbent material effect is different, this
Object in embodiment is changed to capreomycin, remaining condition is constant, and the permeability of record capture front and back object is shown in Table one.
Influence of one different condition of table to the permeability of the ochracin in corn
Claims (7)
1. the preparation method of ochracin adsorbent material in a kind of corn, which is characterized in that including by tetrabutylammonium chloride, sulfuric acid
Calcination obtains after sodium and polyacrylamide-tetraethylenepentamine grafting chelating gel mixing；
The temperature of the calcination is 120~150 DEG C；
Tetrabutylammonium chloride, sodium sulphate and polyacrylamide-tetraethylenepentamine grafting chelating gel mass ratio are 1:7:2.
2. the preparation method of ochracin adsorbent material in corn according to claim 1, which is characterized in that the calcination
Time be 2h, powdery granule object is obtained after calcination；
Then powdery granule object is obtained to ochracin adsorbent material in the corn after vacuum dried.
3. the preparation method of ochracin adsorbent material in corn according to claim 2, which is characterized in that described is true
The dry temperature of sky is 20~40 DEG C, and the vacuum drying time is 24~48h.
4. the preparation method of ochracin adsorbent material in corn according to claim 1,2 or 3, which is characterized in that institute
The method stated is specifically: by sodium sulphate and tetrabutylammonium chloride, being mixed to get two phase aqueous extraction system, then in aqueous two-phase extraction body
Polyacrylamide-tetraethylenepentamine grafting chelating gel is added in system and obtains gel mixture, gel mixture calcination obtains powder
Last shape particulate matter；
Then powdery granule object is obtained to ochracin adsorbent material in the corn after vacuum dried.
5. ochracin adsorbent material in a kind of corn, which is characterized in that the adsorbent material uses any right of claim 1-4
It is required that the preparation method is prepared.
6. application of the ochracin adsorbent material for ochracin absorption in corn in corn described in claim 5.
7. application according to claim 6 is specifically used for corn using ochracin adsorbent material in corn of the invention
It is corn: water: adsorbent material=4:8:1 that the method for middle ochracin absorption, which includes: mass ratio, stands 20min at 26 DEG C.
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Application publication date: 20190219 |