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Method for detecting bisphenol compounds and derivatives of bisphenol compounds based on extraction technology of metal organic framework nanomaterials

A metal-organic framework and nanomaterial technology, applied in the field of detection, can solve the problems of weak adsorption and the inability of the adsorbent to meet the analysis requirements.

Active Publication Date: 2019-04-16
WENZHOU MEDICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Generally speaking, for the same type of organic matter, the adsorption between traditional nanomaterials and polar organic compounds is weaker than that of less polar organic compounds, so traditional adsorbents cannot meet the analysis requirements

Method used

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  • Method for detecting bisphenol compounds and derivatives of bisphenol compounds based on extraction technology of metal organic framework nanomaterials
  • Method for detecting bisphenol compounds and derivatives of bisphenol compounds based on extraction technology of metal organic framework nanomaterials
  • Method for detecting bisphenol compounds and derivatives of bisphenol compounds based on extraction technology of metal organic framework nanomaterials

Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0032] Synthesize NH first 2 -MIL-101(Fe). Add FeCl to 60mL DMF solution 3 ·6H 2 O (19.75mmol, 5.338g) and NH 2 - BDC (10.0 mmol, 1.812 g), the mixture was magnetically stirred for 10 min, then transferred to a stainless steel autoclave with a PTFE liner of 100 mL, and heated at 110° C. for 24 h. After cooling to room temperature, the suspension was transferred to a 100mL plastic centrifuge tube, centrifuged at 7000rpm for 5min to collect a brownish black solid product, which was fully washed with DMF to remove unreacted NH 2 -BDC, washed three times with ultrapure water and ethanol, and finally vacuum-dried at 60 °C for 6 h to obtain activated NH 2 -MIL-101(Fe).

[0033] At 77K liquid nitrogen temperature, through N 2 Adsorption and desorption experiments, analysis of NH 2 - Surface area and pore structure of MIL-101(Fe). NH 2 - N of MIL-101(Fe) 2 The adsorption / desorption isotherm results are as follows figure 2 shown. According to BET and BJH method fitting cal...

Embodiment 2

[0048] The experimental process is as shown in Example 1, except that the amount of extractant is 30 mg, the ultrasonic extraction time is 2.0 min, the elution solvent is 400 μL of methanol, the elution time is 1.0 min, and the pH of the sample is in the range of 2.0-6.0.

[0049] Experimental results:

[0050] The correlation coefficient R of the linear equation of BPs 2 Between 0.9986 and 0.9997; when the signal-to-noise ratio S / N=3, the lowest detection limit is 0.016~0.131μg L -1 ; When the signal-to-noise ratio S / N=10, the quantification limit is 0.05~0.44μg L -1 . The linear ranges of bisphenol compounds and bisphenol derivatives are 0.5~200μg L -1 , 0.25~200μg L -1 .

[0051] In order to detect the stability of the method, the inventors measured the recovery data of the method during the day and within the day, and each detection setting was high (50 μg L -1 ), medium (20μg L -1 ) and low (5μg L -1 ) three concentration levels, the same batch of samples was test...

experiment example

[0053] Experimental reagents: Water samples were collected from different regions in Wenzhou, China. Among them, the river water samples came from the Wenruitang River, the seawater samples came from the coastal area near Yanting Town, Cangnan County, and the tap water samples were collected directly from the laboratory of Wenzhou Medical University. Each water sample was filtered through a 0.45 μm PES filter and stored in a clean glass bottle at 4°C. The above samples were placed at room temperature before use.

[0054] After each type of water sample was grouped, a known amount of BPs was added to the water sample, and the concentration of the standard BPs added was 0, 5 μg L -1 , 20 μg L -1 and 50 μg L -1 .

[0055] Experimental process: The experimental process is as shown in Example 1, the differences are: the amount of extractant is 30 mg, the ultrasonic extraction time is 2.0 min, the elution solvent is 400 μL of methanol, the elution time is 1.0 min, and the pH of ...

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Abstract

The invention provides a method for detecting bisphenol compounds and derivatives of the bisphenol compounds based on extraction technology of metal organic framework nanomaterials. The nano materialis NH2-MIL-101 (Fe) material, and the bisphenol compounds and the derivatives thereof are in a log Kow range of 1.17-3.96, and are called BPS. The method comprises the following steps: S1, adsorbent NH2-MIL-101 (Fe) is added into a sample containing the BPS, the PH value of the sample is adjusted within the range of 2.0 to 7.0, and ultrasonic treatment is carried out for 1.5min to 5.0min so as toobtain the ultrasonic liquid; S2, centrifugal treatment is carried out on ultrasonic liquid obtained in the step S1 to obtain liquid A, and liquid B is obtained after supernate M of the liquid A is removed; S3, after the liquid B obtained in the step S2 is subject to vortex elution for 1.0-5.0min by using an eluent, liquid C is obtained, supernate N of the liquid C is collected, and the eluent isone of methanol, acetonitrile and acetone; and S4, after constant volume is carried out on the supernate N in the step S3, chromatographic analysis and quantification is made.

Description

technical field [0001] The invention relates to the technical field of detection, in particular to a method for using metal-organic framework material-based dispersed micro-solid-phase extraction technology to obtain bisphenol compounds and derivatives thereof Background technique [0002] Metal Organic Frameworks (MOFs), also known as porous coordination polymers (Porous Coordination Polymers, PCPs), are crystals with a highly ordered three-dimensional structure, composed of metal ions (clusters or secondary structural units (SBUs)) and organic Ligands (linkers) self-assemble through coordination bonds to form a network skeleton structure. MOFs have ultra-high specific surface area, up to 10400m 2 g -1 , while the specific surface area of ​​general nanomaterials is much lower than this value. In addition, MOFs also have uniformly structured cavities with specific pore sizes (about 0.3–10 nm), and ultra-low densities (as low as 0.13 g cm -3 ) and thermal stability (about...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/062
Inventor 周佩佩王学东刘伟高曼王慧利李艳艳
Owner WENZHOU MEDICAL UNIV
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