Method for rapidly detecting biogenic amine by thin layer chromatography in one step
A technology of thin-layer chromatography and biogenic amines, applied in measuring devices, analysis materials, instruments, etc., can solve the problems of long preheating equilibrium and analysis time, immature technology, and few complete sets of equipment, etc., to shorten the detection time , detection time is shortened, the effect of easy operation
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Embodiment 1
[0047] Embodiment 1: the preparation of activated silica gel
[0048] Accurately weigh 10g of 200-300 mesh silica gel imported from Merck, Germany, first make a suspension with 50ml DMSO, then add 20ml of epichlorohydrin, shake well; accurately weigh 1.6g of sodium hydroxide, dissolve it in 100ml of deionized water Prepare a 0.4mol / L NaOH solution; finally add 100ml 0.4mol / L NaOH solution to the above-mentioned silica gel activation solution; put the silica gel activation system into a constant temperature shaker at 30°C with a rotation speed of 180rpm for 8 hours, after the activation is completed, filter Remove the liquid system and wash the medium with copious amounts of deionized water until the pH of the filtrate is less than 8.
[0049] Take 30mL of ammonia water with a concentration of 25% and 120mL of deionized water, mix and prepare 5% ammonia water as the activation solution; accurately weigh 10g of epoxy activated silica gel and place it in a 250ml Erlenmeyer flask,...
Embodiment 2
[0051] Embodiment 2: the preparation of activated silica gel
[0052] Accurately weigh 10g of 100-200 mesh domestic silica gel, first make a suspension with 125ml DMSO, then add 60ml of phenoxypropylene oxide, shake well; accurately weigh 3.2g of sodium hydroxide, dissolve it in 100ml of deionized water 0.8mol / L NaOH solution; finally, add 100ml 0.8mol / L NaoH solution to the above silica gel activation solution; put this silica gel activation system into a constant temperature shaker at 35°C and a speed of 180rpm to react for 11 hours, after the activation is completed, filter out the liquid system, And wash the medium with a large amount of deionized water until the pH of the filtrate is less than 8.
[0053] Take 90mL of chloramine with a concentration of 25% and 135mL of deionized water, mix and prepare 10% chloramine as an activation solution system; accurately weigh 10g of epoxy activated silica gel and place it in a 500ml Erlenmeyer flask, add 225mL of 10% chloramine, I...
Embodiment 3
[0055] Embodiment 3: the preparation of activated silica gel
[0056] Accurately weigh 10g of 200-300mesh silica gel imported from Merck, Germany, first make a suspension with 200ml DMSO, then add 100ml of epichlorohydrin, shake well; accurately weigh 4.8g of sodium hydroxide, dissolve in 100ml of deionized water Prepare 1.2mol / L NaOH solution; finally add 100ml 1.2mol / L NaOH solution to the above-mentioned silica gel activation solution; put this silica gel activation system in a constant temperature shaker at 40°C with a rotation speed of 180rpm for 14h, after the activation is completed, filter Remove the liquid system and wash the medium with copious amounts of deionized water until the pH of the filtrate is less than 8.
[0057] Take 180mL of ethylenediamine with a concentration of 25% and 120mL of deionized water, mix and prepare 15% ethylenediamine as an activation solution system; accurately weigh 10g of epoxy-activated silica gel and place it in a 500ml Erlenmeyer fla...
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