Preparation method and application of bacitracin bonded type chromatographic packing
A bacitracin and chromatographic stationary phase technology, applied in the field of chromatographic separation, can solve the problems such as no bond between bacitracin and silica gel, limited choice of mobile phase, etc. Effect
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example 1
[0033] (1) Silanization of carrier silica gel
[0034] Add 3g of activated silica gel and 60mL of anhydrous toluene into a 100mL two-necked flask, ultrasonically disperse the silicon spheres evenly, add 2.5mL of 3-aminopropyltriethoxysilane dropwise while stirring in an ice bath, and reflux at 90°C under nitrogen protection After cooling to room temperature for 24 hours, wash with anhydrous toluene and methanol three times respectively, and dry under vacuum at 40°C to obtain 3-aminopropyl silica gel;
[0035] (2) Synthesis of bonded bacitracin-based chromatography stationary phase
[0036]Take 2.5g of the above dried 3-aminopropyl silica gel, add 50mL of anhydrous toluene, sonicate for 5 minutes, quickly add 2.5mL of hexamethylene diisocyanate under ice bath conditions, reflux at 70°C for 4h under nitrogen protection, and cool to room temperature Finally, remove the solvent and hexamethylene diisocyanate, add 80mL of anhydrous pyridine solution containing 0.8g bacitracin, ref...
example 2
[0038] (1) Silanization of carrier silica gel
[0039] Add 5g of activated silica gel and 120mL of anhydrous toluene into a 250mL two-necked flask, ultrasonically disperse the silicon spheres evenly, add 2.5mL of 3-aminopropyltriethoxysilane dropwise while stirring in an ice bath, and reflux at 125°C under nitrogen protection 4h, after cooling to room temperature, wash with anhydrous toluene and methanol three times respectively, and dry under vacuum at 40°C to obtain 3-aminopropyl silica gel;
[0040] (2) Synthesis of bonded bacitracin-based chromatography stationary phase
[0041] Take 2.5g of the above dried 3-aminopropyl silica gel, add 50mL of anhydrous toluene, sonicate for 5 minutes, quickly add 2.5mL of hexamethylene diisocyanate under ice bath conditions, reflux at 85°C for 2h under nitrogen protection, and cool to room temperature Finally, remove the solvent and hexamethylene diisocyanate, add 80mL of anhydrous pyridine solution containing 0.8g bacitracin, reflux at...
Embodiment 3
[0048] Take 2.0 g of the stationary phase filler obtained in Example 2, and fill it in a 100×4.6 mm I.D. stainless steel column by the homogenization method, and the column packing pressure is 60 MPa. The resulting bacitracin-bonded column.
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