Needle filter solid-phase extraction device for metal organic framework filler

A metal-organic framework and extraction device technology, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of shortening the extraction time, achieve good extraction effect, recyclable cost, and convenient operation

Pending Publication Date: 2020-12-15
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Technical problem: In order to overcome the deficiencies in the prior art, the present invention provides a metal-organic framework filled needle filter solid-phase extraction device, which can

Method used

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  • Needle filter solid-phase extraction device for metal organic framework filler
  • Needle filter solid-phase extraction device for metal organic framework filler
  • Needle filter solid-phase extraction device for metal organic framework filler

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0031] Example 1 Preparation of MIL-101 (Cr) needle filter as filler and its extraction application

[0032] 1. Synthesis of MIL-101 (Cr): 800 mg of chromium nitrate nonahydrate, 332 mg of terephthalic acid, 9.6 mL of water and 0.1 mL of hydrofluoric acid (40%) were sequentially added to a 30 mL reaction kettle polytetrafluoroethylene liner middle. After the ultrasonic mixing was uniform, the inner tank was sealed with a stainless steel sleeve, and the reaction was carried out at 220 °C for 8 h. After the reaction, when the reaction kettle was lowered to room temperature, the solution was transferred to a 50 mL centrifuge tube, and centrifuged at 10,000 rpm for 10 min to discard the supernatant. The lower solid was washed several times with DMF to ensure that the washing solution was colorless, clear and transparent to remove the terephthalic acid and metal salt solution in the pores, and the MIL-101(Cr) solid was collected by centrifugation; then washed with about 15 mL of a...

Example Embodiment

[0039] Example 2 NH 2 -Preparation of MIL-101(Cr)-filled needle filter and its extraction application

[0040] NH 2 -Synthesis of MIL-101(Cr): 800mg Cr(NO 3 ) 3 ·9H 2 O, 360mg 2-aminoterephthalic acid, 200mg NaOH and 15mL deionized water were mixed evenly, transferred to a 50mL polytetrafluoroethylene reactor, reacted at 150°C for 12h, and the solution was transferred to a 50mL centrifuge after the reactor was lowered to room temperature The tube was centrifuged at 10,000 rpm for 10 min and the supernatant was discarded. The solid in the lower layer was repeatedly washed with DMF several times to remove most of 2-aminoterephthalic acid, and then washed three times with about 15 mL of absolute ethanol to replace the residual DMF reagent.

[0041] The remaining steps are the same as steps 2-6 in Example 1.

[0042] The result is as image 3 As shown in B, compared with the dispersive solid phase extraction, the recovery rates of the three target compounds increased from 6...

Example Embodiment

[0043] Embodiment 3 MOF-5 is the preparation of filler needle filter and its extraction application

[0044] Synthesis of MOF-5: Dissolve 0.50g of terephthalic acid in 80mL of DMF, sonicate to dissolve, then add 1mL of triethylamine; take another 1.70g of zinc acetate dihydrate and dissolve in 100mL of DMF, ultrasonicate until completely dissolved, add the above The phthalic acid solution was stirred at room temperature for 4 h, and centrifuged at 12,000 rpm for 15 min. The obtained solid was washed three times with dichloromethane and methanol, respectively, and the solid was collected by centrifugation, and was vacuum-dried at 60 °C overnight.

[0045] The remaining steps are the same as steps 2-6 in Example 1.

[0046] The result is as image 3 As shown in C, compared with the dispersive solid phase extraction, the recovery rates of the three target compounds increased from 2.23% to 5.02% to 13.22% to 56.31%.

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Abstract

The invention relates to a needle filter solid-phase extraction device for a metal organic framework filler, and belongs to the technical field of analytical chemistry sample pretreatment. According to the invention, a metal organic framework dispersion liquid is filled into a needle filter to prepare a solid phase extraction filter head, and a miniaturized solid phase extraction method taking a metal organic framework as an adsorbent and taking the needle filter as an extraction container is developed on the basis of solid phase extraction and adsorbent filling micro-extraction. According tothe method, estrogen can be rapidly enriched through pi-pi action, electrostatic adsorption, space matching and other actions, compared with traditional distributed solid-phase extraction, the extraction time is shortened, the use amount of an extraction agent is reduced, the operation steps are simplified, solid-liquid separation is facilitated, and the device has practical application value.

Description

technical field [0001] The invention relates to a metal-organic framework filler needle filter solid-phase extraction device, which belongs to the technical field of analytical chemical sample pretreatment. Background technique [0002] Environmental estrogens (EEs), also known as exogenous estrogens, are the most diverse category of environmental endocrine disruptors, mainly including natural estrogens and synthetic estrogens. Natural estrogens mainly There are Estradiol (E2), Estrone (Estrone, E1), Estriol (E3), and synthetic estrogens mainly include Ethinylestradiol (EE2), Diethylstilbestrol (DES) , Bisphenol A (Bisphenol A, BPA), etc. Most environmental estrogens have stable chemical properties and a long half-life. They are difficult to decompose in nature and organisms, and the degradation rate is slow. It takes a long time to be excreted from the body. After being enriched in the organism through the food chain, etc., it leads to its toxic accumulation. , resulting ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06B01D15/20
CPCG01N30/02G01N30/06B01D15/206G01N2030/062
Inventor 张毅邓鑫雨王文龙
Owner JIANGNAN UNIV
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