Method for purifying capsaicin monomer by utilizing reverse-phase resin
A technology of reverse phase resin and capsaicin, applied in the separation/purification of carboxylic acid amide, organic chemistry, etc., can solve the problems of unfavorable large-scale industrial production, small processing capacity, expensive equipment, etc. Large, efficiency-enhancing effect
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Embodiment 1
[0019] (1) Concentrate 200mL of the crude capsaicin obtained by the two-phase method under reduced pressure and put it on the pretreated D101 macroporous resin column. The column volume is 120mL, and the capsaicin monomer contained in it is 0.17g as determined by liquid phase. First use 25% (volume ratio) ethanol solution to elute impurity 2BV, then use 70% (volume ratio) ethanol solution to elute capsaicin substances, and 3BV is eluted in total. A total of 2.5 BV of the effluent was collected rich in capsaicin, and the recovery rate of capsaicin was determined by liquid phase to be 96%, and the purity was 34%.
[0020] (2) Concentrate 250mL of the collected capsaicin-rich solution under reduced pressure and put it on a reverse phase resin SKP-10 (particle size 40μm) column with a column volume of 50mL and a sample volume of 0.16g. Use 25% ethanol solution Elute 2BV, 65% ethanol solution gradient elution 4BV, collect the eluate with a fractional collector, combine the effluent...
Embodiment 2
[0023] (1) Concentrate 250mL of the crude capsaicin obtained from the two-phase method under reduced pressure and put it on the pretreated D101 macroporous resin column. First use 30% (volume ratio) ethanol solution to elute impurity 2BV, and then use 65% (volume ratio) ethanol solution to elute capsaicin substances, and 4BV is eluted in total. A total of 3.5 BV of effluent was collected rich in capsaicin, and the recovery rate of capsaicin was determined by liquid phase to be 93%, and the purity was 30%.
[0024] (2) Concentrate the collected capsaicin-rich solution under reduced pressure and put it on a reversed-phase resin SKP-10 (particle size 40 μm) column with a column volume of 50 mL and a sample volume of 0.186 g, wash with 20% ethanol solution Remove 2BV, 55% ethanol solution gradient elution 6BV, collect the eluate with a fractional collector, combine the effluents rich in capsaicin monomer and dihydrocapsaicin monomer respectively, and obtain the liquid phase purity...
Embodiment 3
[0027] (1) Concentrate 275mL of the crude capsaicin obtained from the two-phase method under reduced pressure, and put it on the pretreated D101 macroporous resin column. The column volume is 120mL, and the capsaicin monomer contained in it is 0.22g as determined by liquid phase. First use 20% (volume ratio) ethanol solution to elute the impurity 3BV, then use 60% (volume ratio) ethanol solution to elute capsaicin substances, and 4BV is eluted in total. A total of 3.5 BV of effluent was collected rich in capsaicin, and the recovery rate of capsaicin was determined by liquid phase to be 93%, and the purity was 37%.
[0028] (2) Concentrate the collected capsaicin-rich solution under reduced pressure and put it on a reverse phase resin SKP-10 (particle size 40 μm) column with a column volume of 50 mL and a sample volume of 0.20 g, wash with 30% ethanol solution Remove 3BV, gradient elution of 5BV with 60% ethanol solution, collect the eluate with a fractional collector, combine ...
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