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
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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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