A kind of separation and extraction method of squalene in mixed tocopherols
An extraction method and technology for tocopherol, applied in the field of separation and extraction of squalene, can solve the problems of insignificant extraction effect, small separation scale, difficulty in regeneration of adsorbents, etc., so as to improve adsorption and separation effects, and ensure purity and recovery rate. , the effect of improving the efficiency of scale utilization
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Embodiment 1
[0033] Take 70g of 100-200 mesh coarse-pore silica gel, add a small amount of n-hexane, fill it into the chromatographic column, elute the compacted silica gel with n-hexane 3 times the volume of the chromatographic column, and mix 5g of 50% mixed tocopherol and n-hexane by 2 : 1 (m / m) to dissolve and load the sample. After the sample is loaded, it is first eluted with 3 times the volume of n-hexane, and then eluted with a mixed solvent of n-hexane and ethyl acetate that is 3 times the volume of the chromatography column. The volume ratio of ethyl acetate is 15:1. The eluate was collected in sections and concentrated to obtain the squalene product with a content of 92.56% and a yield of 87.7%. The silica gel column was washed and regenerated with 2 times the volume of methanol.
Embodiment 2
[0035] Take 70g of 100-200 mesh coarse-pore silica gel, add a small amount of cyclohexane, fill it into the chromatographic column, elute the compacted silica gel with cyclohexane 3 times the volume of the chromatographic column, and mix 6.5g of 50% mixed tocopherol with cyclohexane Dissolve hexane at a ratio of 2:1 (m / m), add 5g of silica gel and stir evenly, then add to the top of the silica gel column, first elute with 3 times the volume of cyclohexane, then use 3 times the volume of the chromatography column with cyclohexane and A mixed solvent of ethyl acetate was used for elution, and the volume ratio of cyclohexane to ethyl acetate was 10:1. The eluate was collected in sections and concentrated to obtain the squalene product with a content of 90.28% and a yield of 84.6%. The silica gel column was washed and regenerated with 2 times the volume of ethyl acetate.
Embodiment 3
[0037]Take 100g of 100-200 mesh coarse-pore silica gel, add a small amount of petroleum ether, fill it into the chromatography column, elute the compacted silica gel with petroleum ether 3 times the volume of the chromatography column, and mix 7g of 30% mixed tocopherol and petroleum ether by 2 : 1 (m / m) to dissolve and load the sample. After the sample is loaded, it is eluted with 3 times the volume of petroleum ether, and then eluted with a mixed solvent of petroleum ether and ethyl acetate that is 3 times the volume of the column. Petroleum ether and ethyl acetate The volume ratio of ethyl acetate is 12:1. The eluate was collected in sections and concentrated to obtain the squalene product with a content of 90.8% and a yield of 86.6%. The silica gel column was washed and regenerated with 2 times the volume of methanol.
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