Carbonyl compound affinity chromatography medium and preparation method thereof
A technology for carbonyl compounds and chromatographic media, which is applied in the field of preparation of chromatographic media, and achieves the effects of simple procedure, simple operation and high yield.
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Embodiment 1
[0029] The affinity chromatography medium was prepared by taking methyl nonanone in Houttuynia cordata as an example of carbonyl compounds.
[0030] 1. Take an appropriate amount of silica gel for column chromatography, soak it with 3 times the amount of 6.0mol / L hydrochloric acid for about 40 minutes, filter it with suction, wash it with deionized water, and dry it in a constant temperature drying oven at 100-120°C for about 1 hour, then set it to dry Save in the device for backup;
[0031] 2. Take about 50g of the above-mentioned dried silica gel and put it into a three-neck bottle, add about 100mL of buffer solution (PH4.0~6.0) and about 2.0mL of r-glycidyl etheroxypropyl trimethoxysilane dropwise, at 105~120 React in an oil bath at ℃ for about 90 minutes, and filter out the product;
[0032] 3. Put the above-mentioned filtrate in an oil bath at 55-65°C, hydrolyze it with 0.1-0.2 mol / L sulfuric acid for about 5 hours, and then filter it with suction. The filter cake is fir...
Embodiment 2
[0036] Compared with Example 1, the only difference is that the method described in this example includes the following steps:
[0037] 1. Take an appropriate amount of silica gel for column chromatography, soak it with 2 times the amount of 8.0mol / L hydrochloric acid for about 30 minutes, filter it with suction, wash it with deionized water, and dry it in a constant temperature drying oven at 100°C for about 1 hour, then put it in a desiccator Save for later use;
[0038] 2. Put 50g of dried silica gel into a three-neck bottle, add about 100mL of buffer solution (PH4.0) and about 2.0mL of γ-aminopropyltriethoxysilane dropwise, and react in an oil bath at 120°C for about 60min. filter out the product;
[0039] 3. Put the above-mentioned filtrate in an oil bath at 55°C, hydrolyze it with 0.1mol / L sulfuric acid for about 6 hours, and filter it with suction. The filter cake is washed with distilled water first, and then washed with methanol solution to obtain the activated produ...
Embodiment 3
[0042] Compared with Example 1, the only difference is that the method described in this example includes the following steps:
[0043]1. Take an appropriate amount of silica gel for column chromatography, soak it with 4 times the amount of 4.0mol / L hydrochloric acid for about 50 minutes, filter it with suction, wash it with deionized water, and dry it in a constant temperature drying oven at 120°C for about 0.5 hours, then put it in a desiccator Save it for later use;
[0044] 2. Take 50g of dried silica gel and put it in a three-necked bottle, add about 100mL of buffer solution (PH 6.0) and about 2.0mL of r-glycidyl etheroxypropyl trimethoxysilane dropwise, and react in an oil bath at 105°C for about 120min , filter out the product;
[0045] 3. Put the above-mentioned filtrate in an oil bath at 65°C, hydrolyze it with 0.2moL / L sulfuric acid for about 4 hours and filter it with suction, wash the filter cake with distilled water first, and then wash it with methanol solution ...
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