Method for separating and purifying 6-gingerol
A technology for separation and purification of gingerol, applied in the field of natural medicine, can solve the problems of long operation time, expensive packing, low separation efficiency, etc., and achieve the effects of good quality of finished products, easy operation and high output
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Embodiment 1
[0033] (1) Preliminary separation by silica gel column chromatography
[0034] Use 300g of commercial ginger supercritical fluid extract as raw material, mix the sample with 200g of 100-200 mesh column chromatography silica gel, use 100-200 mesh column chromatography with 2kg of silica gel as the stationary phase, gradient elution, and the polarity of the eluents in sequence Petroleum ether: ethyl acetate = 12: 1, petroleum ether: ethyl acetate = 9: 1 and petroleum ether: ethyl acetate = 6: 1, collected petroleum ether: ethyl acetate = 6: 1 fraction, TLC test combined , and evaporated to dryness on a rotary evaporator to obtain 16.5 g of crude 6-gingerol, with a yield of 5.5%. Its purity is above 65% (HPLC test, area normalization method).
[0035] (2) Refined by silica gel column chromatography
[0036] Mix the 6-gingerol crude product obtained in the previous step, use 200-300 mesh chromatography silica gel as the stationary phase, the amount of silica gel used is 20 times...
Embodiment 2
[0043] (1) Preliminary separation by silica gel column chromatography
[0044]Using 250g of commercial ginger supercritical fluid extract as raw material, 200g of 100-200 mesh column chromatography silica gel as a sample, 1.5kg of 100-200 mesh column chromatography silica gel as a stationary phase, gradient elution, and the polarity of the eluent Petroleum ether: ethyl acetate = 12:1, petroleum ether: ethyl acetate = 9:1 and petroleum ether: ethyl acetate = 6:1, collected petroleum ether: ethyl acetate = 6:1, TLC inspection Combined and evaporated to dryness on a rotary evaporator to obtain about 12 g of crude 6-gingerol with a yield of 4.8%. Its purity is above 65% (HPLC test, area normalization method).
[0045] (2) Refined by silica gel column chromatography
[0046] Mix the 6-gingerol crude product obtained in the previous step, use 200-300 mesh chromatography silica gel as the stationary phase, the amount of silica gel used is 15 times that of the 6-gingerol crude produ...
Embodiment 3
[0053] (1) Preliminary separation by silica gel column chromatography
[0054] Use commercial ginger supercritical fluid extract 100g as raw material, mix sample with 60g silica gel for 100-200 mesh column chromatography, use 1.0kg silica gel for column chromatography with 100-200 mesh as stationary phase, gradient elution, eluent polarity Petroleum ether: ethyl acetate = 12:1, petroleum ether: ethyl acetate = 9:1 and petroleum ether: ethyl acetate = 6:1, collected petroleum ether: ethyl acetate = 6:1, TLC inspection Combined and evaporated to dryness on a rotary evaporator to obtain the crude product of 6-gingerol. It is about 6.5g, the yield is 6.5%, and its purity is above 65% (HPLC test, area normalization method).
[0055] (2) Preparative HPLC purification
[0056] Dissolve the crude 6-gingerol obtained in the previous step with an appropriate amount of methanol, filter it through a 0.45 μm microporous membrane, and purify it by HPLC using Angilent 1100 series. The mobi...
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