Method for purifying capsaicin monomer by utilizing reverse-phase resin

Abstract

The invention relates to the technical field of separation and purification of natural functional ingredients, and particularly discloses a method for purifying a capsaicin monomer by utilizing a reverse-phase resin. The method comprises the following steps: (1) carrying out preliminary purification on a crude capsaicin product obtained by virtue of an aqueous two-phase method by utilizing a macroporous resin; (2) further carrying out purification on the capsaicin by utilizing the novel reverse-phase resin; (3) crystallizing. The method has the beneficial effects that compared with reverse-phase carbon-18 silica gel fillers, the novel reverse-phase resin disclosed by the invention is low in price, low in column pressure and large in adsorption capacity; the whole process is simple and easy to operate and less in investment; meanwhile, a toxic organic solvent is not adopted, so that the production cost is greatly lowered and the purification efficiency is improved. The method is suitable for industrial production.

Description

(1) Technical field

[0001] The invention relates to the technical field of separation and purification of natural functional components, in particular to a method for purifying capsaicin monomer with a reversed-phase resin. (2) Background technology

[0002] The spicy ingredients in capsicum fruit are a class of capsaicinoids mainly capsaicin, which are: capsaicin, dihydrocapsaicin, nordihydrocapsaicin, homocapsaicin and p-methyl capsaicin, p-methyl capsaicin, p- Methyl capsaicin chain, p-methyl capsaicin saturated chain hydrocarbon, p-tolyl capsaicin, etc., among which capsaicin is the main one, and capsaicin and dihydrocapsaicin account for about 90% of the total above. Capsaicin has pharmacological effects such as analgesia, anti-inflammatory, appetite-stimulating, digestion-improving, antibacterial and insecticidal, and selectivity to neurotransmitters. However, some phenolic substances in crude capsaicin can antagonize the effect of capsaicin on nerve skin, so this cr...

Examples

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 ...

(1) Technical field

[0001] The invention relates to the technical field of separation and purification of natural functional components, in particular to a method for purifying capsaicin monomer with a reversed-phase resin. (2) Background technology

[0002] The spicy ingredients in capsicum fruit are a class of capsaicinoids mainly capsaicin, which are: capsaicin, dihydrocapsaicin, nordihydrocapsaicin, homocapsaicin and p-methyl capsaicin, p-methyl capsaicin, p- Methyl capsaicin chain, p-methyl capsaicin saturated chain hydrocarbon, p-tolyl capsaicin, etc., among which capsaicin is the main one, and capsaicin and dihydrocapsaicin account for about 90% of the total above. Capsaicin has pharmacological effects such as analgesia, anti-inflammatory, appetite-stimulating, digestion-improving, antibacterial and insecticidal, and selectivity to neurotransmitters. However, some phenolic substances in crude capsaicin can antagonize the effect of capsaicin on nerve skin, so this cr...

Examples

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 ...