Method for separating and purifying bergamottin from Zaoxiang pomelo oil cell layer
A technology for the separation and purification of bergamot, applied in organic chemistry, etc., can solve the problems of waste of resources, discarded pomelo peel, environmental pollution, etc., and achieve the effects of short production cycle, high recovery rate, and guaranteed accuracy
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Embodiment 1
[0019] Embodiment 1: the present invention carries out the screening determination of influence factor by following test
[0020] 1. Selection of purification materials
[0021] Freeze-dry the collected oil cell layers of 7 pomelo species and grind them into fine powder with a grinding jar. Accurately weigh a certain amount of freeze-dried powder, use petroleum ether (60-90°C) to ultrasonically extract twice at a solid-to-liquid ratio of 1:20, filter and combine the two filtrates, evaporate the filtrate to dryness, and then dissolve the obtained extract in An appropriate amount of chromatographic methanol is used for HPLC analysis of bergamot. HPLC mobile phase includes pure water (A) and chromatographic acetonitrile (B), using 0-1min: 10% B, 1-5min: 10-80% B, 5-10min: 80% B, 10-12min: 80-95 %B,12-15min:95%B,15-19min:95-10%B,19-21min:10%B gradient elution, flow rate is 1ml / min, stationary phase is Waters C18 analytical column (4.6×250 mm, 5 μm), the column temperature is ...
Embodiment 2
[0033] The operating method of the separation and purification bergamot element of the present invention is carried out according to following three steps:
[0034] see figure 1 , (1) Weigh 80g of pomelo oil cell layer freeze-dried powder, add petroleum ether (60-90°C) and ultrasonically extract twice at a solid-to-liquid ratio of 1:20, filter and combine the two filtrates, and put them on a rotary evaporator Evaporate to dryness to obtain the medicinal extract, mix the sample with an appropriate amount of silica gel, evaporate to dryness and make loading powder, pack the column according to the ratio of 1g:50g between the loading amount and the silica gel consumption, add petroleum ether-acetic acid to the silica gel column after adding the loading powder Ethyl ester (13:1) solution eluted bergamot, combined the eluent containing bergamot, and evaporated to dryness on a rotary evaporator at 40°C to obtain 74.6 mg of crude silica gel extract, the content of bergamot in the cru...
Embodiment 3
[0037] The operating method of the separation and purification bergamot element of the present invention is carried out according to following three steps:
[0038] see figure 1, (1) Weigh 90g of pomelo oil cell layer freeze-dried powder, add petroleum ether (60-90°C) and ultrasonically extract twice at a solid-to-liquid ratio of 1:20, filter and combine the two filtrates, and put them on a rotary evaporator Evaporate to dryness to obtain the medicinal extract, mix the sample with an appropriate amount of silica gel, evaporate to dryness and make loading powder, pack the column according to the ratio of 1g:50g between the loading amount and the silica gel consumption, add petroleum ether-acetic acid to the silica gel column after adding the loading powder Ethyl ester (13:1) solution eluted bergamot, combined the eluent containing bergamot, and evaporated to dryness on a rotary evaporator at 40°C to obtain 83.2 mg of crude silica gel extract, the content of bergamot in the crud...
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