Method for extracting and purifying sequoyitol by using solvent circulation reflux
A reflux extraction and seclitaxel technology, which is applied in ether separation/purification, organic chemistry, medical raw materials derived from gymnosperm subphylum, etc., can solve the problems of difficult separation and purification, good water solubility and low yield, etc. Improve product quality and output, reduce production costs, and the effect of simple and reliable methods
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Embodiment 1
[0028] The raw material is the branches and leaves of Taxus yunnanensis, which can also be used, leaves, bark, wood and roots, and the water content is less than 15%. 100kg of raw materials are crushed into 20-30 mesh coarse particles or coarse powder by a pulverizer. Evenly fill the crushed branches and leaves into the extraction container, add 4-5 times the amount of 80% ethanol for extraction three times each time, or use 10-50% ethanol for extraction, so that the liquid level of the extraction solvent is higher than The surface of the pulverized material is preferably 5-10cm, the temperature: room temperature - reflux temperature, the time of each extraction is about 3-8 hours, and the extraction liquid is combined and concentrated. Using a rotary evaporator, the combined extracts are concentrated at a temperature lower than 80 degrees and vacuum: normal pressure--0.09MPa to form a concentrated extract of Taxus chinensis in the form of a liquid extract. After weighing, add...
Embodiment 2
[0036]100kg of raw material of Taxus chinensis dry branch and leaf, raw material processing is the same as embodiment 1, with methanol, can adopt acetone, isopropanol or acetonitrile leaching three times, also can adopt the methanol of water content 10-50%, or acetone, or isopropanol leaching Extraction, adding 4-5 times of extraction solvent each time, preferably 5-10cm higher than the surface of the ground material with the extraction solvent liquid level, temperature and extraction time are the same as in Example 1, and the extraction solution is combined and concentrated. Concentrate the combined extracts into liquid extracts at a temperature of 20-80° C. and vacuum degree: normal pressure-0.09 MPa to obtain a concentrated extract of Taxus chinensis. After weighing, add 0.5-2 times (W / W) diatomaceous earth, silica gel or activated carbon inert filler to the concentrated yew extract under stirring, mix thoroughly and dry in the air or below 100 °C . Add 3-5 (w / w) times the...
Embodiment 3
[0038] Taxus yunnanensis raw material bark 800kg, raw material processing is the same as embodiment 1, adds 80% acetone leaching three times of 4-5 times of amount at every turn, is advisable with extraction solvent liquid level higher than pulverized material surface 5-10cm, extraction temperature, The time and collection of the extract were the same as in Example 1. Concentrate the combined extracts at a temperature lower than 80 degrees and vacuum: normal pressure - 0.09 MPa to form a concentrated extract of Taxus chinensis in the form of a liquid extract. After weighing, add 0.5-2 times (W / W) diatomaceous earth, silica gel or activated carbon inert filler to the concentrated yew extract under stirring, mix thoroughly and dry in the air or below 100 °C . Add 3-5 (w / w) times the amount of methanol to the dry concentrate as a dissolving agent for at least 2 times of reflux to dissolve, let stand, filter while hot or pour out the clear liquid, collect the reflux liquid, conce...
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