CN111778015A - Zr4+Induced metal organic gel fluorescent switch sensing material and preparation method and application thereof - Google Patents
Zr4+Induced metal organic gel fluorescent switch sensing material and preparation method and application thereof Download PDFInfo
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
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Abstract
The invention discloses Zr4+The induced metal organic gel fluorescent switch sensing material and the preparation method and the application thereof, wherein the method comprises the following steps: a1 preparation of DMF and H2O into the reaction vessel and then shaken thoroughly until complete mixing, DMF: H2The volume ratio of O is 7: 3; a2 adding BTC into the above reaction vessel, sonicating the reaction vessel for 20 seconds until the ligand BTC in the system is completely dissolved, then ZrCl4Adding into the mixed solvent; ZrCl4The molar ratio of BTC is 1: 4; a3, putting the reaction system into an ultrasonic instrument, and carrying out ultrasonic treatment at 80 ℃ for 30 minutes to form white columnar gel. The novel fluorescent switch sensing platform constructed by the invention can selectively detect ARG through charge transfer effect and rapidly detect and remove CrO in water through energy resonance transfer and chemical adsorption effect4 2‑。
Description
Technical Field
The invention belongs to the field of analytical chemistry, and discloses a method for preparing a high-purity high2O as a solvent to construct a Zr4+An induced metal-organic hydrogel fluorescence switch sensing platform for stably and selectively detecting ARG and rapidly detecting and removing CrO in water4 2-。
Background
Arginine (ARG) is a semi-essential basic amino acid containing multiple N binding sites in the human body and plays an important role in wound healing, promoting urea synthesis and excretion, and maintaining acid-base balance and sperm motility. ARG is commonly used in food products as a flavoring or nutritional supplement, added to edible products. Although ARG has many benefits for the human body, it is not suitable for people with different constitutions or levels of health due to its specific requirements for food. For example, people with allergic conditions, diabetes or hepatic insufficiency are not suitable for consumption. Therefore, there is a need to find a sensor that can detect arginine in food. Serious ionic contamination of wastewater is considered one of the most disturbing environmental problems, especially the impact on human health. In particular Cr (VI), e.g. CrO4 2-It is extremely harmful because of its high toxicity. It accumulates in the human body even at low concentrations, resulting in genetic defects, corrosiveness and strong carcinogenicity, and there is therefore an urgent need to find a method or material which can simultaneously detect and remove toxic ions.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides Zr4+Induced metal organic gel fluorescent switch sensing material, preparation method and application thereof, and application thereof in stable and selective detection of ARG and rapid detection and removal of CrO in water4 2-. The novel fluorescent switch induction platform shows good selectivity and stability to arginine in the linear range of 0-2.5. mu.M, with a limit of detection (LOD) of 2.99 ppb. Direct application of Zr-MOG' hydrogel after ARG detection to CrO4 2-The stimulus response in the aqueous phase shows excellent selectivity and high efficiency in the linear range of 0.5-10.2 μ M, with a detection limit as low as 5.2 ppb.
Zr4+The preparation method of the induced metal organic gel fluorescent switch sensing material is characterized by comprising the following steps:
a1 preparation of DMF and H2O into the reaction vessel and then shaken thoroughly until complete mixing, DMF: H2The volume ratio of O is 7: 3;
a2 BTC was added to the above reaction vessel, the reaction vessel was sonicated for 20 seconds until the ligand BTC in the system was completely dissolved, and then ZrCl was added4Adding into the mixed solvent; ZrCl4The molar ratio of BTC is 1: 4;
a3, putting the reaction system into an ultrasonic instrument, and carrying out ultrasonic treatment at 80 ℃ for 30 minutes to form white columnar gel.
Zr prepared by the preparation method4+The induced metal organic gel fluorescence switch sensing material captures Zr-MOG' hydrogel of ARG, and the fluorescence efficiency of the material is obviously amplified; at the same time, CrO4 2-Has obvious quenching effect on the fluorescence efficiency of the Zr-MOG' hydrogel capturing the ARG.
The application of the metal organic gel fluorescent switch sensing material is used as a fluorescent switch sensing material.
The application of the metal organic gel fluorescent switch sensing material is used as an Arginine (ARG) detection sensor.
The application of the metal organic gel fluorescent switch sensing material as CrO4 2-Detecting sensors or in removing CrO4 2-The use of (1).
The invention has the following advantages:
1. the analyte can be detected in water;
2. novel fluorescence switch sensing platform for selectively detecting ARG through charge transfer and rapidly detecting and removing CrO in water through energy resonance transfer and chemical adsorption4 2-；
3. Lower detection limit compared to other reported methods;
4. under the interference of other amino acids, metal ions and other substances, the detection effect is still not influenced.
Drawings
FIG. 1 is a pictorial representation of a gel;
FIG. 2 scanning electron microscope and transmission electron microscope pictures of the gel;
FIG. 3(a) XPS summary profile of gel; (b) infrared absorption spectrum of the gel; (c) c1s orbital spectrum of Zr-MOG gel; (d) c1s orbital spectrum of Zr-MOG' gel;
FIG. 4(a) a spectrum of Zr-MOG selective trapping food additive; (b) fluorescence enhancement efficiency of the Zr-MOG gel; (c) and (d) concentration titration spectra of the Zr-MOG gel; (e) a linear fit plot of the Zr-MOG gel; (f) non-linear fit plot of Zr-MOG gel.
FIG. 5(a) stimulus response experiment of different heavy metal ions to Zr-MOG' hydrogel; (b) quenching efficiency of the heavy metal ions on Zr-MOG' hydrogel fluorescence quenching; (c) cr (VI) concentration titration experiment spectrogram of the gel; (d) linear fit curve of Cr (VI) to gel stimulus response
FIG. 6(a) absorption spectra of Zr-MOG' xerogel adsorbing Cr (VI) at different concentrations; (b) langmuir adsorption isotherm fit curve of Zr-MOG' xerogel adsorption Cr (VI); (c) absorption spectrum chart of absorption kinetics of Zr-MOG' xerogel for absorbing Cr (VI); (d) a line graph of adsorption kinetics of Zr-MOG' xerogel adsorbing Cr (VI); (e) interference experiments of Zr-MOG' xerogel adsorbing Cr (VI); (f) optical photographs before and after the Zr-MOG' xerogel adsorbs Cr (VI).
Detailed Description
The present invention will be described in detail with reference to specific examples.
The present invention selects the following food additives as target analytes for conducting selectivity experiments: ARG, SRL, XLT, AA, LAC, CA, TAR, GLY, ALA, FRU, DHAS.
The synthesized Zr-MOG is selectively detected to ARG.
The specific implementation steps for preparing Zr-MOG are as follows:
1. DMF (7mL) and H2O (3mL) was transferred to a glass vial and then shaken thoroughly until mixed completely.
2. BTC (0.051g, 0.025mmol) was added to a glass vial. The vial was sonicated for 20 seconds until the ligand in the system was completely dissolved. Then ZrCl is added4(0.023g, 0.1mmol) was added to the mixed solvent.
3. Finally, the reaction system was placed in an ultrasonic apparatus and ultrasonically heated (80 ℃) for 30 minutes to form a white columnar gel (FIG. 1). The hydrogel yield is
Detection of Zr-MOG as fluorescent Probe for ARG:
various food additives were added to the reaction system prior to gel formation (between steps 1-2 above) to explore their ability to respond to Zr-MOG stimulation. Interestingly, no other target analytes produced a significant fluorescence enhancement effect on Zr-MOG except ARG (FIG. 4 a). Furthermore, the fluorescence amplification efficiency of ARG is as high as 87.9% with other variables fixed (fig. 4b), indicating its excellent ability to turn "on" in a fluorescent switch.
To further explore the ability of the Zr-MOG hydrogel to detect trace ARG, fluorescence emission spectra of the Zr-MOG hydrogel were obtained after mixing AGR with different concentrations of hydrogel precursor solutions. As shown in FIGS. 4c and 4d, the fluorescence intensity of the hydrogel gradually increased with increasing ARG concentration. Concentration and fluorescence intensity of 0-2.5. mu.M (R)20.993) showed a good linear fit. They show a good non-linear fit trend (R) over a wide concentration range (0-25.6mM)20.982). This may be due to limited Zr4+The binding sites lead to a restriction of the Zr-MOG hydrogel to capture ARG. LOD 3 sigma/Ksv(σ is the mostStandard deviation of low signal, KsvRepresenting the approximate slope of a linear fit curve) was used to calculate the hydrogel detection limit for ARG. Hydrogels have certain advantages over other reports in synthesis and modification time, synthesis cost, detection range and detection limit (2.99ppb in the 0-2.5 μ M range).
Ion fluorescence detection
Since the hydrogel after trapping ARG has many naked N element binding sites, the ARG-trapped Zr-MOG 'hydrogel can be directly used for the ion stimulus response experiment, and the hydrogel containing 0.03mM arginine (Zr-MOG') can be directly used for the subsequent ion assay. Zr-MOG' (2.5mL) was dispersed in 5mL of H2O, then stirred vigorously for 30 minutes. The obtained dispersion was finally used for fluorescence sensing experiments.
Zr-MOG' (500. mu.L) was transferred to a centrifuge tube containing a solution of various ions (2.5mL) and the tube was shaken for 30 minutes. After the hydrogel and the ions are completely mixed, the hydrogel can be used for subsequent stimulation response experiments of the ions to the gel.
CrO4 2-And (3) analysis: the target analyte was (0.1mM) several ionic solutions. The method comprises the following steps: cd [ Cd ]2+，Na+，Ce3+，Nd3+，Er3+，Tb3+，F-，Ac-，SO4 2-，HSO4 -，CO3 2-，HCO3 -，H2PO4 -，HPO4 2-，PO4 3-And CrO4 2-. Fluorescence spectra were recorded by excitation at 370 nm.
According to FIGS. 5a and 5b, except for CrO4 2-Almost completely quenches the fluorescence of the Zr-MOG' hydrogel, other ions are weakened to different degrees, and CrO4 2-Has the highest quenching efficiency, which can reach 98.5 percent (figure 5 b). Thus, the Zr-MOG' hydrogel is paired with CrO in comparison with other ions4 2-And is more sensitive.
To understand CrO further4 2-The Zr-MOG 'water was investigated for its stimulatory response to the Zr-MOG' hydrogelFluorescence intensity of gel with CrO4 2-The concentration varied from an increase of 0-500. mu.M (FIG. 5 c). The quenching effect can be quantified by using the Stern-Volmer (SV) equation: i is0/I＝1+KSV[M]In which I0And I is the luminous intensity of the Zr-MOG' hydrogel and added with CrO with different concentrations4 2-Luminescence intensity of Zr-MOG' hydrogel of solution, [ M]Is CrO4 2-In a molar ratio ofSVIs the quenching constant. Clearly, in the low concentration range, the SV plot is almost linear (fig. 5 d). Zr-MOG' hydrogel vs CrO4 2-Highest K ofSVValue 0.06429 × 106M-1For CrO4 2-The detection limit of (2) was 5.2 ppb. Compared with the MOF and other related materials and sensors, the material has excellent quenching capacity. Illustrating its excellent ability to turn "off" in a fluorescent switch.
It will be understood that modifications and variations can be made by persons skilled in the art in light of the above teachings and all such modifications and variations are intended to be included within the scope of the invention as defined in the appended claims.
Claims (5)
1. Zr4+The preparation method of the induced metal organic gel fluorescent switch sensing material is characterized by comprising the following steps:
a1 preparation of DMF and H2O into the reaction vessel and then shaken thoroughly until complete mixing, DMF: H2The volume ratio of O is 7: 3;
a2 BTC was added to the above reaction vessel, the reaction vessel was sonicated for 20 seconds until the ligand BTC in the system was completely dissolved, and then ZrCl was added4Adding into the mixed solvent; ZrCl4The molar ratio of BTC is 1: 4;
a3, putting the reaction system into an ultrasonic instrument, and carrying out ultrasonic treatment at 80 ℃ for 30 minutes to form white columnar gel.
2. Zr produced by the production method according to claim 14+The induced metal organic gel fluorescent switch sensing material is characterized by capturingThe fluorescence efficiency of Zr-MOG' hydrogel of ARG is obviously amplified; at the same time, CrO4 2-Has obvious quenching effect on the fluorescence efficiency of the Zr-MOG' hydrogel capturing the ARG.
3. Use of the metal organogel fluorescent switch sensing material according to claim 1 as a fluorescent switch sensing material.
4. Use of the metal organogel fluorescent switch sensing material according to claim 1, characterized in that it is used as an Arginine (ARG) detection sensor.
5. The use of the metal organogel fluorescent switch sensing material of claim 1 as CrO4 2-Detecting sensors or in removing CrO4 2-The use of (1).
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| CN112940277A (en) * | 2021-02-19 | 2021-06-11 | 安徽大学 | Formic acid rare earth metal organic framework complex and preparation method and application thereof |
| CN113004315A (en) * | 2021-02-09 | 2021-06-22 | 安徽大学 | Histidine-triggered organic hydrogel fluorescent probe and preparation method and application thereof |
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| CN110358109A (en) * | 2019-08-14 | 2019-10-22 | 安徽大学 | A kind of luminous Zr-MOG metal organogel and its synthetic method |
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| WO2008092628A1 (en) * | 2007-01-30 | 2008-08-07 | Universität Zu Köln | Method for the production of biocompatible hybrimers for optical applications |
| US20140343413A1 (en) * | 2011-11-25 | 2014-11-20 | Danmarks Tekniske Universitet | Formulation of solid nano-sized particles in a gel-forming system |
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| CN113004315A (en) * | 2021-02-09 | 2021-06-22 | 安徽大学 | Histidine-triggered organic hydrogel fluorescent probe and preparation method and application thereof |
| CN113004315B (en) * | 2021-02-09 | 2023-05-26 | 安徽大学 | Histidine-triggered organic hydrogel fluorescent probe and preparation method and application thereof |
| CN112940277A (en) * | 2021-02-19 | 2021-06-11 | 安徽大学 | Formic acid rare earth metal organic framework complex and preparation method and application thereof |
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