Superficially-porous core-shell-structured silica gel microspheres and preparation method and application thereof
A technology of core-shell structure and silica gel microspheres, which is applied in the field of analytical chemistry, can solve the problems of poor reproducibility and long time, and achieve the effects of short preparation time, good reproducibility and simple preparation method
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Embodiment 1
[0025] Add 10 g of spherical silica gel with a particle size of 5 μm to 10 mL of 35 wt% H 2 SiF 6 In the aqueous solution, stir for 2h; then add 5mL of water and 6mL of 0.1mol·L -1 h 3 BO 3 Solution, mix well; first put the mixed solution in a vacuum environment for 1h, then shake it in a shaker at 40°C for 24h, then filter the reacted mixed solution with a sand core funnel, and dry the filtered solid at 120°C Dry, then place the dried product in a muffle furnace, raise it to 200°C at a rate of 140°C / min, and keep it for 2h, and then get the surface porous core-shell structure silica gel microspheres, that is, SiO 2 @SiO 2 ;
[0026] Then put the prepared surface porous core-shell silica gel in the reaction kettle, add 8mL of octadecyltrimethoxysilane and 20mL of anhydrous toluene, react at 130°C for 12h, cool, and filter with suction. The solid was washed successively with toluene, acetone, and methanol, and dried at 45°C for later use to obtain octadecyl-bonded SiO 2 ...
Embodiment 2
[0028] Add 10 g of spherical silica gel with a particle size of 5 μm to 10 mL of 35 wt% H 2 SiF 6 In the aqueous solution, stir for 16h; then add 5mL of water and 6mL of 0.1mol·L -1 h 3 BO 3 Solution, mix evenly; first put the mixed solution in a vacuum environment for 1h, then shake it in a shaker at 40°C for 12h, then filter the reacted mixed solution with a sand core funnel, and dry the filtered solid at 120°C Dry, then place the dried product in a muffle furnace, raise it to 200°C at a rate of 140°C / min, and keep it for 2h, and then get the surface porous core-shell structure silica gel microspheres, that is, SiO 2 @SiO 2 ;
[0029] Then put the prepared surface porous core-shell silica gel in the reaction kettle, add 8mL of aminopropyltrimethoxysilane and 20mL of anhydrous toluene, react at 130°C for 12h, cool, and filter the solid Wash with toluene, acetone, and methanol in sequence, and dry at 45°C for later use to obtain amino-bonded SiO 2 @SiO 2 .
Embodiment 3
[0031] Octadecyl bonded to SiO 2 @SiO 2 Packed in a 50mm×4.6mm (i.d.) liquid chromatography column, and then used for 5 standard peptide sample mixtures (CRGRGRGR-594.73kDa, SPVLAEDPSEGEE-1269.21kDa, CFRGL-594.73, CFRGLRGFRG-1381.61, AngitotensinⅡ-1046.18) The chromatographic separation obtained a good separation effect.
[0032] Chromatographic conditions: solvent A is 0.1% TFA aqueous solution, solvent B is acetonitrile / 0.1% TFA. The mobile phase gradient program is (t represents time (min), for example: t 20 means 20 minutes after injection): t 0 , 20% B; t 20 , 90% B; flow rate: 0.2 mL / min; sample injection volume: 20 μL; detection wavelength: 215 nm; column temperature: 50°C.
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