A chemically selective nanoprobe derived from high selection and high sensitivity enrichment and its preparation method and application
A nano-probe, high-selectivity technology, applied in the preparation of test samples, etc., can solve the problems of unfavorable target compound detection, low target compound recovery rate, poor mass spectrometry ionization efficiency of derivatized groups, etc., and achieve good application. Prospect, high recovery rate, good selectivity effect
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Embodiment 1
[0023] Implementation example 1.mSiO 2 Synthesis of @azobenzene-COOH chemically selective nanoprobes: the whole synthesis reaction is divided into five steps,
[0024] The first step: Synthesis of 3-4-((4-aminophenyl)diazenyl)-4-(dimethylamino)benzoic acid and d 4 -3-4-((4-aminophenyl)diazenyl)-4-(dimethylamino)benzoic acid: 2.76g of 4-nitroaniline was dissolved in 600mL of methanol / water (2:1v / v ) in the mixture. Under the condition of ice bath, add the nitrous acid synthesized by 1.38g sodium nitrite and 3.5mL 37wt% concentrated hydrochloric acid, after reacting for 1 hour, the mixed solution is transferred to 400mL containing 3.3g of 4-(dimethylamino)benzoic acid In methanol solution, the reaction was carried out in an ice bath for 6 hours. The product was suction-filtered, washed with water and then dried under vacuum at 60°C to obtain a mixture containing 4-(dimethylamino)-3-((4-nitrophenyl)diazenyl)benzoic acid. The mixture was passed through SiO 2 Purified by chrom...
Embodiment 2
[0029] Example 2. 100 μL of 500ng / mL 10 kinds of amine mixed standard or 5 μg / mL phenolic hydroxyl mixed standard was diluted to 1 mL with ACN and added to 40 mg of activated mSiO 2 In the @azobenzene-COOH probe, after vortex shaking for 5 minutes, the nanoparticles were centrifuged at 14000rpm / min for 10min and then washed three times with 80% ACN, then the nanoparticles were ultrasonically dispersed in 300μLACN and then added with 300μL 0.2M Na 2 S 2 o 4 Vortex for 1 h, then add 300 μL ethyl acetate to extract three times. The extracts were combined, lyophilized and redissolved in 40 μL of 80% ACN for LC / MS analysis. Add 100μL 0.5M sodium carbonate / sodium bicarbonate buffer solution with pH=9.4 to 100μL 500ng / mL 10 kinds of amine mixed standard or 5μg / mL phenolic hydroxyl mixed standard, add 100μL 20mg / mL dansyl chloride at 60℃ Under reaction 1h. Subsequently, 30 μL of 0.5 M methylamine solution was added to react for 0.5 h at 60°C. The product solution was directly ana...
Embodiment 3
[0030] Example 3. Selective enrichment and LC-MS analysis of amines in derivatized serum.
[0031] (1) Serum pretreatment. After thawing, 20 μL of serum was centrifuged at 14000 rpm / min with an ultrafiltration tube (3000 Da cutoff), and 200 μL of water was added repeatedly to wash the residue three times until the solution was completely centrifuged. The filtrate was passed directly through a Phenomenex 96-well plate to remove phospholipids. The filtrate was lyophilized and redissolved in 1 mL of ACN. 40 mg of chemically selective nanoprobes were sequentially activated with 200 μL of 10 mM HATU, DIPEA and NHS for 2 minutes, then washed three times with 1 mL of 80% acetonitrile / water and twice with 1 mL of acetonitrile, and then added reconstituted serum for extraction. Sonicate and vortex for 5 minutes, centrifuge at 14,000 rpm / min for 10 minutes, wash three times with 1 mL of 80% acetonitrile / water, then disperse in 300 μL of acetonitrile and an equal volume of 0.2 mM Na 2...
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