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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

Inactive Publication Date: 2008-08-20
昆明万宝集源生物科技有限公司
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AI Technical Summary

Problems solved by technology

As a natural product, there are many problems in the extraction and purification of Seclitaxel: 1. The content of Seclitaxel in raw materials is lower than that of ordinary natural products, and the content of different plants and different parts varies greatly
2. There are many impurities and isomers similar in structure to Seclitaxel in the raw material, with good water solubility and high polarity. It is difficult to separate and purify without using conventional separation methods
3. In the separation process, it is not easy to control the separation and purification process with thin-layer chromatography, ultraviolet and other monitoring means, which increases the difficulty of separation and purification
4. The existing Seclitaxel extraction and purification process has high cost, low purity and low yield

Method used

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  • Method for extracting and purifying sequoyitol by using solvent circulation reflux

Examples

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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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Abstract

The invention relates to a method for refluxing, extracting and purifying sequoyitol by a solvent, comprising the following steps: taxus raw material is grinded; extracting and concentrating are carried out to obtain taxus concentrated extract; the taxus concentrated extract is concentrated to fluid extract and mixed; inert filler is added and the mixture is dried after mixed evenly, and sequoyitol dry concentrate is obtained; the sequoyitol dry concentrate is refluxed and dissolved at least two times, and kept on standing and return flow is collected, concentrated, cooled, and kept on standing, and solid or precipitate is collected; sequoyitol coarse product is obtained after being dried; a dissolving agent is added to reflux and dissolve, the mixture is filtered, and the return flow is collected, concentrated, cooled, kept on standing, crystallized in low temperature, and filtered, and crystal is collected; water is added into the sequoyitol crystal to heat and mix until the crystal is dissolved; one among lower alcohol, acetone and acetonitrile is added, and mixed evenly, temperature is kept, the mixture is kept on standing, cooled, crystallized in low temperature, and filtered, the crystal is collected, and the process of crystallizing is repeated for at least three times; sequoyitol crystal is dried, samples are inspected and sequoyitol high-purity product with content more than or equal to 99 percent is obtained. The method for refluxing, extracting and purifying the sequoyitol by the solvent is characterized by using the solvent to reflux and extract, separate and purify the sequoyitol from taxus raw material. The method for refluxing, extracting and purifying the sequoyitol by the solvent is advanced in technique, high in reproducibility, high in yield rate, high in purity, simple and reliable in method, strong in operation, and low in production cost, and is especially suitable for large-scaled industrial production.

Description

technical field [0001] The invention relates to a method for extracting paclitaxel from yew and other plant materials, in particular to a method for extracting and purifying paclitaxel by solvent reflux. Background technique [0002] Taxus has extremely high medicinal value, but in addition to the development and utilization of anti-cancer effects, the development of other effects is far from enough. A large amount of Taxus is used in the production of taxane compounds such as paclitaxel and 10-DAB , other functional ingredients wherein are basically not utilized, resulting in a waste of resources. [0003] Sequoyitol is an active ingredient extracted from Taxus chinensis for treating diabetes. English name: Sequoyitol Chemical name: 5-0-methyl-myoinositol (or 5-oxo-methyl-meso-inositol) Molecular formula: C 7 h 14 o 6 Molecular weight: 194.20 Its chemical structure is as follows: [0004] [0005] It is contained in yew bark, branches and leaves, the content is about...

Claims

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Application Information

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IPC IPC(8): C07C43/196C07C41/34A61K36/13A61P3/10
Inventor 张坤平
Owner 昆明万宝集源生物科技有限公司
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