MOF-Cd probe for detecting Fe3+ and antibiotic ceftriaxone sodium in water, preparation method and application thereof

A technology of ceftriaxone sodium and antibiotics, applied in the field of analytical chemistry, can solve problems such as expensive and time-consuming, and achieve the effect of low detection limit

Active Publication Date: 2018-08-21
ANHUI UNIVERSITY
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Problems solved by technology

However, these mechanical methods not only require trained personn

Method used

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  • MOF-Cd probe for detecting Fe3+ and antibiotic ceftriaxone sodium in water, preparation method and application thereof
  • MOF-Cd probe for detecting Fe3+ and antibiotic ceftriaxone sodium in water, preparation method and application thereof
  • MOF-Cd probe for detecting Fe3+ and antibiotic ceftriaxone sodium in water, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Embodiment 1 prepares the specific embodiment of MOF-Cd solution:

[0022] First synthesize the ligand bbi: weigh imidazole (0.05-0.1moL) and sodium hydroxide (0.05-0.1moL) and dissolve them in DMSO (10mL) for 2 hours at 60°C, then weigh 1,4-dichlorobutane (0.025 ~ 0.5moL) was added to the above solution several times, and after the reaction was continued for 2 ~ 3h, the solution was poured into a beaker containing 500mL of ice water and left to stand overnight to obtain a large amount of white needle-shaped product, which was obtained by suction filtration. Let dry and set aside.

[0023] Then weigh bbi (20-40mg), phthalic acid (20-40mg), Cd(NO 3 ) 2 (0.0494~0.1g) in DMA (10mL), stirred and dissolved, placed in a polytetrafluoroethylene liner, and reacted at 80°C for 40~48h to obtain a colorless transparent single crystal. figure 1 is the obtained MOF-Cd structure.

[0024] Add 20 mg of single crystal to a centrifuge tube of 5 mL DMSO for ultrasonic dispersion, and...

Embodiment 2

[0026] Example 2: MOF-Cd as a fluorescent probe for Fe 3+ detection

[0027] Add 150 μL of metal ion solution to the MOF-Cd solution and add Fe respectively 3+ , Eu 3+ , La 3+ , Y 3+ , Ba 2+ , Ni 2 + ,Co 2+ , Ag + , Zn 2+ ,Sr 2+ , Cd 2+ , K + , Mn 2+ , Na + , Li + , Mg 2+ , Ca 2+ . image 3 Middle Fe 3+ The fluorescence of MOF-Cd solution decreased obviously.

[0028] In MOF-Cd solution, when Fe 3+ When the amount of MOF-Cd increased from 0 μL to 40 μL, the fluorescence intensity of MOF-Cd decreased monotonously and sharply, Figure 4 with Fe 3+ With the increase of concentration, the fluorescence intensity of MOF-Cd solution was gradually quenched. This indicates that MOF-Cd can be used as a fluorescent probe for Fe 3+highly sensitive. The fluorescence quenching efficiency can be quantitatively explained by the Stern-Volmer (SV) equation, and the detection limit can also be calculated: where I 0 is the fluorescence intensity before the analyte, I is ...

Embodiment 3

[0031] Example 3: MOF-Cd as a fluorescent probe for the detection of ceftriaxone sodium

[0032] Add 15 μL of antibiotic solution to the MOF-Cd solution, add SXT (sulfamethoxazole), MTR (metronidazole tablets), CFM (cefixime), CED (cefradine), CEC (cefaclox), CSU respectively (ceftiamidine), FOX (cefoxitin sodium), ATM (aztreonam), GEN (gentamycin sulfate), AZM (azithromycin), AMX (amoxicillin), ERY (erythromycin ethyl succinate) , AMK (acamicin), CRO (ceftriaxone sodium), PEN (penicillin sodium), AZL (azithromycin lactobionate), LIN (lincomycin hydrochloride). Figure 7 The fluorescence of MOF-Cd significantly decreased by ceftriaxone sodium.

[0033] In MOF-Cd solution, when the amount of ceftriaxone sodium increased from 0 μL to 7 μL, the fluorescence intensity of MOF-Cd decreased monotonously and sharply, Figure 8 with Fe 3+ With the increase of concentration, the fluorescence intensity of MOF-Cd solution was gradually quenched. By calculation, the detection limit is ...

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Abstract

The invention discloses a MOF-Cd probe for detecting Fe3+ and antibiotic ceftriaxone sodium in water, a preparation method and application thereof. The preparation method comprises the following steps: preparation of ligand bbi: fetching 0.05-0.1 moL of imidazole and 0.05-0.1moL of sodium hydroxide; dissolving the imidazole and the sodium hydroxide in DMSO for reacting for 2h at 60 degrees; then weighing 0.025-0.5moL of 1,4-dichlorobutane; adding the 1,4-dichlorobutane into the solution for multiple times; subjecting the solution to a sustained reaction for 2-3h; pouring the solution into a beaker containing 500 mL of ice water; performing still standing overnight; obtaining a large amount of white needle-like products; performing suction filtration to obtain white products, drying the white products for standby application; fetching and placing 20-40 mg of bbi, 20-40 mg of phenylenediacetic acid, 0.0494-0.1g of Cd(NO3)2 in DMA; stirring; dissolving and placing the mixture in a polytetrafluoroethylene liner; subjecting to a reaction for 40-48h at 80 degrees; and obtaining colorless transparent single crystals, which is the MOF-Cd probe. An analyte can be detected in water, and theeffect of detection is still not affected under different pH conditions and interference of other metal ions and antibiotics.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and specifically designs a method that uses bbi=1,4-bis(2-methylimidazol-1-yl)butane and phthalic acid as ligands, and uses Cd(NO 3 ) 2 4H 2 O as a metal node to construct a new MOF-Cd material with stable fluorescence properties, which can be used for the detection of Fe in water with high selectivity, high sensitivity and high stability 3+ and the antibiotic ceftriaxone sodium. Background technique [0002] With increasing public health and water quality concerns, there is an increasing need for contamination detection in wastewater. Metal ion pollution, which can cause damage and disease to humans and other organisms, has become a serious environmental problem. As an important organic pollutant, antibiotics are widely used to treat bacterial infections in humans and animals. Excessive use of antibiotics has resulted in high concentrations of antibiotic residues in groundwater and surfa...

Claims

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Application Information

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IPC IPC(8): G01N21/64
CPCG01N21/6428G01N2021/6432
Inventor 牛和林邢鹏程吴笛毛昌杰宋吉明
Owner ANHUI UNIVERSITY
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