A novel monosaccharide fluorescence derivatization method and application
A monosaccharide and fluorescent technology, applied in the direction of fluorescence/phosphorescence, chemical instruments and methods, luminescent materials, etc., can solve the problems of a large number of time samples, unreliable sugar quantitative effect, loss, etc.
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Embodiment 1
[0028] Take galactose 0.25g, NaHCO 3 67mg, then add 0.67g of 1,3-bis(2-pyridine)-1,3-propanedione, then add 40ml of methanol aqueous solution (3:1, v / v), mix well, and react overnight at 110°C. After methanol was removed under reduced pressure, it was dissolved in an appropriate amount of water, and further purified by a C18 solid-phase extraction column (elution with 10% acetonitrile) and a silica gel column (10% methanol in chloroform solution).
[0029] The resulting labeled product was assayed by HPLC. Measurement was performed at an excitation wavelength of 330 nm and an absorption wavelength of 390 nm using a C18 reversed-phase column (HyperClone5uODS120A250x4.60 mm).
[0030] HPLC analysis results such as figure 1 As shown, the ESI MS results are as figure 2 shown.
Embodiment 2
[0032] Take D-galactose (D-Galactose), D-mannose (D-Mannose), D-gulose (D-Gulose), D-arabinose (D-Arabinose), D-celery sugar (D-Apiose ), D-xylose (D-Xylose), L-fucose (L-Fucose), L-rhamnose (L-Rhamnose) aqueous solution 8ul (20mM), add 2ul 0.4M sodium bicarbonate aqueous solution, Then add 30ul of 0.1M 1,3-bis(2-pyridine)-1,3-propanedione methanol solution, seal and mix well, then react overnight at 110°C. After the reaction was completed, they were diluted with water to 2 ml, centrifuged at 13000 r / m for 1 minute, and the supernatant was taken for HPLC analysis.
[0033] HPLC analysis results such as image 3 , wherein peak numbers 1-8 are D-galactose, D-gulose, D-mannose, D-arabinose, D-apiose, D-xylose, L-fucose and L - Derivative products of rhamnose.
Embodiment 3
[0035] Weigh 100ug of glycoprotein horseradish peroxidase (HRP), add 40ul 4M trifluoroacetic acid (TFA) aqueous solution, hydrolyze at 115°C for 3 hours, remove TFA by vacuum rotary evaporator, in order to remove TFA as much as possible, add 100ul 50% methanol aqueous solution and spin dry, repeat 3 times. HPLC analysis was performed after labeling with 1,3-bis(2-pyridine)-1,3-propanedione.
[0036] The result is as Figure 4 , where peak numbers 1-4 are derivatives of D-mannose, D-arabinose, D-xylose and L-fucose, respectively.
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