CN111909028A - Preparation method of Eu/Tb (BTC) for detecting AFB1 - Google Patents
Preparation method of Eu/Tb (BTC) for detecting AFB1 Download PDFInfo
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- CN111909028A CN111909028A CN202010859878.6A CN202010859878A CN111909028A CN 111909028 A CN111909028 A CN 111909028A CN 202010859878 A CN202010859878 A CN 202010859878A CN 111909028 A CN111909028 A CN 111909028A
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- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
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Abstract
The invention discloses a preparation method of Eu/Tb (BTC) for detecting AFB1, which comprises the following steps of: 1: 100 terbium salt, europium salt and ligand were added to 6mL of DMF: h2O is 5:1 mixed solvent; carrying out ultrasonic treatment for 20min to form emulsion, then putting the emulsion into a reaction kettle, heating the emulsion in a programmed heating oven to 100 ℃, reacting for 12h, and taking out; the withdrawn reaction was cooled to room temperature and filtered to obtain Eu/Tb (BTC). The method is simple in preparation and low in cost, and the prepared Eu/Tb (BTC) can be used for conveniently and quickly detecting the AFB1 by naked eyes.
Description
Technical Field
The invention relates to the technical field of organic molecule detection, in particular to a preparation method of Eu/Tb (BTC) (europium terbium bimetallic material containing trimesic acid) for detecting AFB 1.
Background
Aflatoxin B1(AFB1), a metabolite produced by fungi in food containing mold, is directly or indirectly introduced into the human food chain through different routes, if it is eaten by mistake, causing serious harm to human beings and the risk of carcinogenesis and death, seriously threatens human health and life safety, and has serious damage to human and animal internal organs, especially liver. It has strong chemical and thermal stability and can be completely destroyed by heating to 230 ℃, so that general cooking processing is not easy to eliminate, and considering that these factors seriously threaten the health of human beings and animals, many countries and regions have established regulations to manage the level of AFB1 in agricultural products to ensure food safety. For example, peanuts, milk, dried fruits and cereals set by the european union have an AFB1 content of up to 2 ppb. It is therefore crucial to develop sensitive analytical techniques for detecting AFB1 to control mycotoxin exposure.
In the prior art, a spectrophotometer and other large-scale precise instruments are used for analyzing organic molecules, but a great challenge exists in how to quickly detect specific small molecules (such as AFB1), and particularly, the prior art does not have such a solution as to realize naked eye detection without a large-scale instrument.
Disclosure of Invention
The invention aims to provide a preparation method of Eu/Tb (BTC) for detecting AFB1, which is simple in preparation and low in cost, and the prepared Eu/Tb (BTC) can be used for conveniently and quickly detecting AFB1 by naked eyes.
The purpose of the invention is realized by the following technical scheme:
a method of making Eu/tb (btc) for detecting AFB1, the method comprising:
step 1, mixing a mixture of a molar ratio of 100: 1: 100 terbium salt, europium salt and ligand were added to 6mL of DMF: h2O is 5:1 mixed solvent;
and 3, cooling the taken reactant to room temperature and filtering to obtain Eu/Tb (BTC).
According to the technical scheme provided by the invention, the method is simple to prepare and low in cost, and the prepared Eu/Tb (BTC) can be used for conveniently and quickly detecting the AFB1 by naked eyes.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on the drawings without creative efforts.
FIG. 1 is a schematic flow chart of a preparation method of Eu/Tb (BTC) for detecting AFB1 according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of the crystal structure of Eu/Tb (BTC) according to an exemplary embodiment of the present invention;
FIG. 3 is a schematic diagram of the fluorescence spectrum of Eu/Tb (BTC) at 254nm according to an exemplary embodiment of the present invention;
FIG. 4 is a schematic diagram of the fluorescence titration of AFB1 with Eu/Tb (BTC) according to an exemplary embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without making any creative effort, shall fall within the protection scope of the present invention.
Referring to the drawings, the embodiment of the present invention will be described in further detail, and fig. 1 is a schematic flow chart of a preparation method of Eu/tb (btc) (europium terbium bimetallic material containing trimesic acid) for detecting AFB1 according to the embodiment of the present invention, wherein the method comprises:
step 1, mixing a mixture of a molar ratio of 100: 1: 100 terbium salt, europium salt and ligand were added to 6mL of DMF: h2O is 5:1 mixed solvent;
in this step, the terbium salt may be Tb (NO)3)3·6H2O; the europium salt can be Eu (NO)3)3·6H2O。
The ligand can be trimesic acid H3 BTC。
and 3, cooling the taken reactant to room temperature and filtering to obtain Eu/Tb (BTC).
After obtaining the Eu/tb (btc), the method further comprises:
preparing a suspension of Eu/Tb (BTC) methanol at a concentration of 0.3mg/mL by using the Eu/Tb (BTC);
and (3) putting 1mM AFB1& methanol solution into the suspension of Eu/Tb (BTC) methanol, and under the irradiation of an ultraviolet lamp at 254nm, changing the original yellow fluorescence of the suspension of Eu/Tb (BTC) methanol into white fluorescence, thereby realizing naked eye detection of AFB 1.
The following describes in detail the procedure of the above preparation method and the naked eye detection of AFB1 by specific examples, in which 4mg of terbium nitrate, 226mg of terbium nitrate and 105mgH are first weighed out3BTC is added to the volume ratio5:1 DMF and H26mL of O mixed solvent;
then carrying out ultrasonic treatment for 20min to obtain emulsion, putting the emulsion into a reaction kettle, heating the emulsion in a programmed heating oven to 100 ℃ for reaction for 12h, and taking out the emulsion; after cooling, the Eu/Tb (BTC) is obtained by room temperature filtration, and as shown in FIG. 2, the Eu/Tb (BTC) crystal structure of the embodiment of the present invention is schematically shown.
The Eu/Tb (BTC) sample obtained in the above is placed in an Edinburgh FS5 fluorescence spectrometer with an excitation wavelength of 254nm and a slit of 0.5, and a schematic diagram of the fluorescence spectrum of Eu/Tb (BTC) at 254nm of an exemplary embodiment of the present invention is shown in FIG. 3.
Then, 0.1mL, 0.2mL, 0.3mL, 0.4mL, 0.5mL, 0.6mL, 0.7mL, 0.8mL, 0.9mL, 1.0mL of AFB1 methanol solution with concentration of 1mM are added to the suspension of 3mLEu/Tb (BTC) methanol to determine the corresponding fluorescence emission spectra, as shown in FIG. 4, the fluorescence of the example Eu/Tb (BTC) to AFB1 titration is shown in FIG. 4: the fluorescence peaks at 487nm, 548nm and 616nm are all increased differently, and the increase of the fluorescence peak at 487nm is most obvious.
Further, 1.0mL of 1mM AFB1 methanol solution was added to 3mL of the material methanol dispersion, and placed under a 254nm ultraviolet lamp, the yellow fluorescence of the original material was clearly seen to change to white fluorescence, thereby realizing naked eye detection of AFB 1.
It is noted that those skilled in the art will recognize that embodiments of the present invention are not described in detail herein.
In conclusion, the method provided by the embodiment of the invention has the advantages that the synthetic raw materials are cheap and easy to obtain, the conditions are simple and mild, the mass preparation is easy, the prepared Eu/Tb (BTC) can visually see the color change from yellow to white to AFB1 under the visual observation, and the method has good potential application value in detecting AFB 1.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (4)
1. A method for preparing Eu/Tb (BTC) for detecting AFB1, said method comprising:
step 1, mixing a mixture of a molar ratio of 100: 1: 100 terbium salt, europium salt and ligand were added to 6mL of DMF: h2O is 5:1 mixed solvent;
step 2, performing ultrasonic treatment for 20min to form emulsion, then putting the emulsion into a reaction kettle, heating the emulsion in a programmed heating oven to 100 ℃ for reaction for 12h, and taking out the emulsion;
and 3, cooling the taken reactant to room temperature and filtering to obtain Eu/Tb (BTC).
2. The method of preparing Eu/Tb (BTC) for detecting AFB1 according to claim 1, wherein in step 1 said terbium salt is Tb (NO)3)3·6H2O; the europium salt is Eu (NO)3)3·6H2O。
3. The method for preparing Eu/Tb (BTC) for detecting AFB1 according to claim 1, wherein said ligand is trimesic acid H in step 13 BTC。
4. The method for preparing Eu/tb (btc) for detection of AFB1 according to claim 1, wherein after obtaining said Eu/tb (btc), said method further comprises:
preparing a suspension of Eu/Tb (BTC) methanol at a concentration of 0.3mg/mL by using the Eu/Tb (BTC);
and (3) putting 1mM AFB1& methanol solution into the suspension of Eu/Tb (BTC) methanol, and under the irradiation of an ultraviolet lamp at 254nm, changing the original yellow fluorescence of the suspension of Eu/Tb (BTC) methanol into white fluorescence, thereby realizing naked eye detection of AFB 1.
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Citations (8)
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| US20080300387A1 (en) * | 2005-11-16 | 2008-12-04 | Basf Se | Organometallic Framework Materials of Transition Group III |
| US20140284829A1 (en) * | 2011-10-04 | 2014-09-25 | Fundació Institut Catalá De Nanociéncia I Nanotecnologia | Method for the preparation of metal organic frameworks |
| CN105949226A (en) * | 2016-06-23 | 2016-09-21 | 哈尔滨工业大学 | Preparation method of europium/cerium-codoped complex fluorescent sensing material and application of fluorescent sensing material in detecting organic small-molecule compounds |
| CN107163069A (en) * | 2017-05-10 | 2017-09-15 | 浙江大学 | The preparation of lanthanide series metal organic framework materials and its method for Visual retrieval chiral enantiomer |
| CN109232619A (en) * | 2018-11-05 | 2019-01-18 | 中山大学 | Multicolor fluorescence material based on rare earth metal organic frame and preparation method thereof and anti-counterfeiting ink application |
| CN110204654A (en) * | 2019-06-12 | 2019-09-06 | 河南工业大学 | Aflatoxin surface imprinted polymer and its application based on HKUST-1 |
| CN111476333A (en) * | 2020-04-02 | 2020-07-31 | 齐鲁工业大学 | L n-MOF-based multicolor heterojunction micro intelligent response photon anti-counterfeiting bar code material, device, preparation and application |
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2020
- 2020-08-24 CN CN202010859878.6A patent/CN111909028B/en active Active
Patent Citations (8)
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| US20080300387A1 (en) * | 2005-11-16 | 2008-12-04 | Basf Se | Organometallic Framework Materials of Transition Group III |
| CN101241131A (en) * | 2008-02-21 | 2008-08-13 | 江苏省原子医学研究所 | Reagent kit for simultaneously detecting ochratoxin A and aspergillus flavus toxin B1 and its detection method |
| US20140284829A1 (en) * | 2011-10-04 | 2014-09-25 | Fundació Institut Catalá De Nanociéncia I Nanotecnologia | Method for the preparation of metal organic frameworks |
| CN105949226A (en) * | 2016-06-23 | 2016-09-21 | 哈尔滨工业大学 | Preparation method of europium/cerium-codoped complex fluorescent sensing material and application of fluorescent sensing material in detecting organic small-molecule compounds |
| CN107163069A (en) * | 2017-05-10 | 2017-09-15 | 浙江大学 | The preparation of lanthanide series metal organic framework materials and its method for Visual retrieval chiral enantiomer |
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