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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

AI Technical Summary

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 quickly enrich estrogen and solve the problems of shortening the extraction time, saving the amount of extractant, Technical issues such as simplified operation steps and easy solid-liquid separation

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

Embodiment 1

[0031] Embodiment 1 MIL-101 (Cr) is the preparation and extraction application of the syringe filter of filler

[0032] 1. Synthesis of MIL-101 (Cr): Add 800mg chromium nitrate nonahydrate, 332mg terephthalic acid, 9.6mL water and 0.1 mL hydrofluoric acid (40%) to a 30mL reactor polytetrafluoroethylene liner in sequence middle. After ultrasonic mixing, put the liner into a stainless steel sleeve and seal it, and react at 220°C for 8 hours. After the reaction was completed, the reaction kettle was cooled to room temperature, the solution was transferred to a 50 mL centrifuge tube, 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 ensure that the washing liquid was colorless, clear and transparent to remove the terephthalic acid and metal salt solution in the channel, and the MIL-101 (Cr) solid was collected by centrifugation; then washed with about 15 mL of absolute ethanol Thr...

Embodiment 2

[0039] Example 2 NH 2 -Preparation of needle filter with MIL-101(Cr) as filler 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 reaction kettle, and reacted at 150°C for 12h. After the reaction kettle was lowered to room temperature, the solution was transferred to a 50mL centrifuge The tube was centrifuged at 10000rpm for 10min and the supernatant was discarded. The solid in the lower layer was repeatedly washed with DMF several times to remove most of the 2-aminoterephthalic acid, and then washed 3 times with about 15 mL of absolute ethanol to replace the remaining DMF reagent. The solid was collected by centrifugation and dried under vacuum at 40°C overnight.

[0041] All the other steps are the same as steps 2-6 of Example 1.

[0042] The result is as image 3 As shown in B, compared wit...

Embodiment 3

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

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

[0045] All the other steps are the same as steps 2-6 of Example 1.

[0046] The result is as image 3 As shown in C, compared with the dispersed solid phase extraction, the recoveries of the three target substances 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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