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Method for separating paclitaxel by utilizing rosin-based bonded silica gel stationary phase

A technology for bonding silica gel and rosin base, which is applied in the field of high performance liquid chromatography, can solve the problems of unsatisfactory separation effect of paclitaxel and its analogs, low column efficiency of chromatographic columns, etc., and achieves increased spatial selectivity and good separation effect. , The effect of high solvent tolerance

Active Publication Date: 2021-02-19
GUANGXI UNIV FOR NATITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the method is simple and reproducible; but its separation effect on paclitaxel and its analogues is not ideal, and the column efficiency of the chromatographic column is low

Method used

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  • Method for separating paclitaxel by utilizing rosin-based bonded silica gel stationary phase
  • Method for separating paclitaxel by utilizing rosin-based bonded silica gel stationary phase
  • Method for separating paclitaxel by utilizing rosin-based bonded silica gel stationary phase

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Experimental program
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Effect test

preparation Embodiment 1

[0034] First put 7.0g of silica gel into aqueous hydrochloric acid solution, reflux for 5 hours under the protection of nitrogen, wash with high-purity water until neutral, and dry in vacuum to obtain the activation of silica gel; then 5.5g of activated silica gel, 50.0g of anhydrous toluene, 5.0g of 3 -(methacryloyloxy)propyltrimethoxysilane was added to a three-necked flask, stirred magnetically, refluxed for 5 hours, washed with toluene and acetone, and dried in vacuum to obtain silica gel modified with silane coupling agent; finally, 5.0 g of disproportionated rosin (β- Dissolve acryloyloxyethyl) ester in ethyl acetate, then add 5.0g of silane coupling agent to modify silica gel, disperse by ultrasonic, add 0.08g of initiator azobisisobutyronitrile, protect with nitrogen, and react at 75°C for 6h to obtain Rosin-based bonded silica stationary phase.

preparation Embodiment 2

[0036] First put 15.0g of silica gel into aqueous hydrochloric acid solution, reflux for 3h under the protection of argon, wash with high-purity water until neutral, and dry in vacuum to obtain the activation of silica gel; then 14.0g of activated silica gel, 70.0g of anhydrous toluene, 15.0g Add (3-mercaptopropyl) trimethoxysilane into a three-necked flask, stir magnetically, reflux for 7 hours, wash with toluene and methanol, and dry in vacuo to obtain a silane coupling agent-modified silica gel; finally, 14.0 g of dehydroabietic acid (β - Dissolve acryloyloxyethyl) ester in butyl acetate, then add 13.0g of silane coupling agent to modify silica gel, disperse by ultrasonic, add 0.15g of initiator dibenzoyl peroxide, and react at 70°C under the protection of argon After 8 hours, a rosin-based bonded silica gel stationary phase was obtained.

preparation Embodiment 3

[0038]First put 25.0g of silica gel into aqueous hydrochloric acid solution, reflux for 8 hours under the protection of nitrogen, wash with high-purity water until neutral, and dry in vacuum to obtain the activation of silica gel; then 23.0g of activated silica gel, 210.0g of anhydrous toluene, 20.0g ( Add 3-mercaptopropyl)triethoxysilane into a three-necked flask, stir magnetically, reflux for 8 hours, wash with toluene and ethanol, and dry in vacuo to obtain silane coupling agent-modified silica gel; In ethyl acetate, add 23.0g silane coupling agent to modify silica gel, ultrasonically disperse, add 0.35g initiator tert-butyl hydroperoxide, and react at 78°C for 8h under nitrogen protection to obtain rosin-based bonded silica gel stationary phase.

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Abstract

The invention discloses a method for separating paclitaxel by utilizing a rosin-based bonded silica gel stationary phase, and belongs to the field of high performance liquid chromatography. The methodcomprises the following steps of: modifying activated silica gel by utilizing a silane coupling agent, reacting the modified silica gel with a polymerizable rosin-based monomer under the condition ofan initiator to form a rosin-based bonded silica gel stationary phase material, setting the parameters of a liquid chromatograph, dissolving a sample to be detected, and introducing the dissolved sample into a chromatographic column filled with the rosin-based bonded silica gel stationary phase material, so as to realize separation, wherein the separation degree of the 10- deacetylated baccatin III and the baccatin III is 3.33-7.74, the separation degree of the baccatin III and the 10-deacetylated paclitaxel is 3.48-13.25, the separation degree of the 10- deacetylated paclitaxel and the cephalotaxine is 2.57-5.49, and the separation degree of the cephalotaxine and the paclitaxel is 1.96-5.34. The method provided by the invention has high separation degree and selectivity on paclitaxel andanalogues thereof, and is simple to operate, high in sensitivity, rapid and efficient.

Description

technical field [0001] The invention belongs to the field of high-performance liquid chromatography, and in particular relates to a method for separating paclitaxel by using a rosin-based bonded silica gel stationary phase. Background technique [0002] Paclitaxel is one of the most effective anticancer drugs for human beings. Paclitaxel has special preventive and treatment effects on esophageal cancer, lung cancer, ovarian cancer, colon cancer and acute leukemia. By exploring methods such as genetic engineering, chemical semi-synthesis, and chemical total synthesis, the cost is relatively high. Extracting, separating and purifying paclitaxel from Taxus chinensis is the main method for preparing paclitaxel. [0003] The roots, bark, branches and leaves of Taxus chinensis contain taxanes (diterpenoids), flavonoids and other substances, among which taxanes are represented by paclitaxel, cephalomannine, 10-deacetyl paclitaxel (Structural analogue of paclitaxel), baccatin Ⅲ, 1...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D305/14B01J20/286B01J20/28B01J20/30B01D15/32
CPCC07D305/14B01J20/286B01J20/28004B01J20/28019B01J20/28083B01J20/28059B01J20/28061B01D15/32
Inventor 李浩雷福厚谢文博易冯梅曾磊
Owner GUANGXI UNIV FOR NATITIES
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