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Method for determining content of salivary acid in serum by using UIO-66-NH2 material

A UIO-66-NH2, sialic acid technology, applied in measurement devices, material separation, analysis of materials, etc., can solve problems such as undiscovered, and achieve the effects of good stability, high extraction capacity and efficiency

Inactive Publication Date: 2016-09-21
QUFU NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, no UIO-66-NH has been found at home and abroad 2 A report on the method of determining the content of sialic acid in serum by materials

Method used

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  • Method for determining content of salivary acid in serum by using UIO-66-NH2 material
  • Method for determining content of salivary acid in serum by using UIO-66-NH2 material
  • Method for determining content of salivary acid in serum by using UIO-66-NH2 material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] UIO-66-NH of the present invention 2 The preparation process of the material is as follows:

[0039] Accurately weigh 3.15g of zirconium tetrachloride (13.5mmol), 2.45g of 2-aminoterephthalic acid (13.5mmol) and 0.24g of water (13.5mmol) into the reactor, and use 489.7g of N,N-dimethyl Dimethylformamide (6.7 mol) was dissolved and magnetically stirred until a transparent solution was formed. The reaction kettle was heated at 120°C for 6 hours, and the crystallization process was kept in a static state. After the reaction, cool, filter, wash, and dry, and the obtained UIO-66-NH 2 The crude product was washed with methanol for 3 days to remove residual DMF in the crystals, and the finally obtained crystals were dried at 60°C. To prevent UIO-66-NH 2 The material absorbs moisture to reduce the activity, and the crystals are sealed and stored.

[0040] The present invention will UIO-66-NH 2 The material was successfully applied to the extraction of sialic acid standard...

Embodiment 2

[0047] The present invention adopts the UIO-66-NH prepared by Example 1 2 The material was successfully applied to the extraction of sialic acid in human normal serum, and the sialic acid was sensitively detected by high performance liquid chromatography.

[0048] Specific steps are as follows;

[0049] (1) Using trifluoroacetic acid to hydrolyze the serum sample, remove the protein and then centrifuge to obtain the serum treatment solution;

[0050] (2) Measure 2mL of serum treatment solution into a 4mL centrifuge tube, then add 9mg of synthetic UIO-66-NH 2 The material was fully extracted by vortex shaking for 6 minutes to obtain the extract, and the supernatant was discarded by centrifugation at 10,000 rpm and 4°C for 10 minutes;

[0051] (3) Add 0.2mL aqueous solution containing 5wt.% acetic acid into the centrifuged test tube, and ultrasonicate for 6min to remove sialic acid from UIO-66-NH 2 Completely eluted in the material;

[0052] (4) Pre-column derivatization of th...

Embodiment 3

[0055] The present invention adopts the UIO-66-NH prepared by Example 1 2 The material was successfully applied to the extraction of sialic acid in human cancer serum, and the sensitive detection of sialic acid was carried out by means of high performance liquid chromatography.

[0056] Specific steps are as follows;

[0057] (1) Using trifluoroacetic acid to hydrolyze the cancer serum sample, remove the protein and then centrifuge to obtain the serum treatment solution;

[0058] (2) Measure 2mL of serum treatment solution into a 4mL centrifuge tube, then add 10mg of synthetic UIO-66-NH 2 The material was fully extracted by vortex shaking for 7 minutes to obtain the extract, and the supernatant was discarded by centrifugation at 5000rpm and 4°C for 15 minutes;

[0059] (3) 0.2mL aqueous solution containing 5wt.% acetic acid was added to the centrifuged test tube, and ultrasonicated for 5min to remove sialic acid from UIO-66-NH 2 Completely eluted in the material;

[0060] ...

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Abstract

The invention belongs to the technical field of application of metal-organic framework composite material, and in particular, relates to a method for determining the content of salivary acid in serum by using a UIO-66-NH2 material. The method comprises the steps: hydrolyzing a serum sample by using trifluoroacetic acid, removing proteins, and then centrifuging to obtain a serum treatment fluid; mixing the serum treatment fluid with the UIO-66-NH2 material, carrying out vortex oscillation extraction, extracting the salivary acid in the serum treatment fluid into the UIO-66-NH2 material, and centrifuging to obtain a salivary acid-containing UIO-66-NH2 material; carrying out ultrasonic elution of the salivary acid-containing UIO-66-NH2 material obtained after centrifugation with an acetic acid aqueous solution, and making the salivary acid completely eluted from the UIO-66-NH2 material, to obtain an eluate; and carrying out precolumn derivatization of the eluate with a fluorescence derivatization reagent, and then carrying out high performance liquid chromatography detection. The method for determining the content of the salivary acid in the serum has the advantages of high selectivity and high sensitivity.

Description

technical field [0001] The invention belongs to the technical field of application of metal-organic framework composite materials, and specifically relates to a method using UIO-66-NH 2 Materials Method for determination of sialic acid content in serum. Background technique [0002] Metal-organic frameworks (MOFs) are a new class of nanoporous materials that are connected by metal ions and organic ligands through coordination bonds. Due to the octahedral structure of MOF materials, it not only has the characteristics of high porosity, large specific surface area, adjustable pore size, and structural diversity, but also shows great thermal and chemical stability in water and organic solutions. It has been widely used in many fields, such as gas adsorption separation, catalysis, drug delivery, biological imaging and other fields. However, the application of MOF materials in the field of analytical chemistry lags far behind other fields. [0003] Sialic acid is a nine-carbon...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/027G01N2030/062
Inventor 夏莲武传香刘丽洁
Owner QUFU NORMAL UNIV
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