Improved process for isolation and purification of paclitaxel from natural sources
A paclitaxel, raw material technology, applied in the improvement field of separation and purification of paclitaxel from natural raw materials, to achieve the effect of reducing production costs
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Embodiment 1
[0126] washing
[0127] 100 kg of dried and ground Canadian yew needles and branches were packed into cotton bags. The bag was placed into a stainless steel tank filled with 400 liters of distilled water. The cotton bag was completely submerged in water for 3 hours at room temperature, and the solution containing water-soluble impurities was drained.
[0128] In practice, this washing process can be repeated once or twice, with the wet needles remaining in the tank through the cotton bag.
[0129] extraction
[0130] Add 250 liters of methanol to the pot with the wet needles and twigs. Extract at room temperature for 16 hours. The extract is pumped through the filter into a second double walled tank. Methanol was distilled by means of hot water at 80°C circulating in a double-walled tank. The recovered methanol is fed into the needle tank for rinsing, and the volume of pure methanol reaches 400 liters at the end. The rinsed methanol is then pumped and distilled until ap...
Embodiment 2
[0140] First chromatographic purification on silica gel at low pressure
[0141] The acetone solution containing paclitaxel and its analogs obtained after removal of resin and pigment in Example 1 was mixed with 500 g of silica gel (230-400 mesh). The silica gel impregnated with the extract is air-dried (or dried under vacuum). The total weight after drying was approximately 900-950 grams, and half of this material was loaded onto a column (142 x 7.6 cm id) containing 2.2 kg of silica gel (230-400 mesh). The silica gel was washed and equilibrated with a mixture of acetone and hexane (35:65%, v / v). With the same solvent, use Dynamax Solvent delivery system for elution. The flow rate for elution at a pressure of 0-30 psi is approximately 100 ml / min. The volume of the solvent mixture was about 40 liters and the fractions were collected in 1 liter batches. HPLC analysis showed 9 to 10 fractions (from No. 26 or No. 27 to No. 35 or No. 36) containing about 0.2 mg / ml to 0.7 mg...
Embodiment 3
[0145] First chromatographic purification on silica gel at low pressure
[0146] The acetone solution containing paclitaxel and its analogs obtained after removing the resin and pigment in Example 1 was mixed with 500 g of silica gel (230-400 mesh). The silica gel impregnated with the extract is air-dried (or dried under vacuum). The total dry weight was approximately 920 grams, and half of this material was loaded onto a column (142 x 7.6 cm id) containing 2.2 kg of silica gel (230-400 mesh). The silica gel was washed and equilibrated with a mixture of acetone and hexane (40:60%, v / v). With the same solvent, use Dynamax Solvent delivery system for elution. The flow rate for elution at a pressure of 0-30 psi is approximately 100 ml / min. The volume of the solvent mixture was about 30 liters and the fractions were collected in 1 liter batches. HPLC analysis showed 7 to 8 fractions (from the 16th or 17th to the 23rd or 24th fraction) containing about 0.1 mg / ml to 0.7 mg / ml...
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