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Method for separating camptothecin and 10-hydroxycamptothecin by adoption of rosin-based macromolecules

A hydroxycamptothecin and rosin-based technology, applied in the field of high performance liquid chromatography, can solve problems that have not been reported, and achieve good permeability, high column efficiency, and good separation effect

Active Publication Date: 2017-04-19
GUANGXI UNIV FOR NATITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] There is no report about the separation of camptothecin and 10-hydroxycamptothecin using a rosin-based polymer chromatographic column

Method used

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  • Method for separating camptothecin and 10-hydroxycamptothecin by adoption of rosin-based macromolecules
  • Method for separating camptothecin and 10-hydroxycamptothecin by adoption of rosin-based macromolecules
  • Method for separating camptothecin and 10-hydroxycamptothecin by adoption of rosin-based macromolecules

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Add 200g of deionized water, 0.4g of sodium lauryl sulfate, and 4.0g of polyvinyl alcohol into a 250mL beaker (the mass ratio of ionized water, sodium lauryl sulfate, and polyvinyl alcohol is 100:0.2:2), Heat to 95°C to completely dissolve the polyvinyl alcohol and sodium lauryl sulfate to obtain an aqueous phase, which is transferred to a water bath to keep the temperature down to 55°C.

[0045] Weigh 3.00g of maleic rosin ethylene glycol acrylate, dissolve it in 50.0g of ethyl acetate, and use ultrasonic waves to promote dissolution. After the crosslinking agent is completely dissolved, add 0.50g of α-methacrylic acid and 1.00g of isooctane in sequence , 0.10g of azobisisobutyronitrile (the mass ratio of functional monomer, crosslinking agent, solvent, porogen, and initiator is 0.5:3:50:1:0.1), ultrasonically oscillated for 10min, dispersed evenly, and obtained oil Mutually.

[0046] Add the prepared oil phase to the water phase (the mass ratio of the oil phase and t...

Embodiment 2

[0050] Add 400g deionized water, 2.00g sodium lauryl sulfate, and 12.00g polyvinyl alcohol into a 500mL beaker (the mass ratio of ionized water, sodium lauryl sulfate, and polyvinyl alcohol is 100:0.5:3), Heat to 95°C to completely dissolve the polyvinyl alcohol and sodium lauryl sulfate to obtain an aqueous phase, which is transferred to a water bath to keep the temperature down to 55°C.

[0051] Weigh 12.00g of maleic rosin ethylene glycol acrylate, dissolve it in 100.00g of ethyl acetate, and use ultrasonic waves to promote dissolution. After the cross-linking agent is completely dissolved, add 3.00g of methyl methacrylate and 5.00g of isooctyl Alkane, 2.00g of azobisisobutyronitrile (the mass ratio of functional monomer, cross-linking agent, solvent, porogen, and initiator is 3:12:100:5:2), ultrasonically oscillated for 10 minutes, dispersed evenly, and prepared oily phase.

[0052] Add the prepared oil phase to the water phase (the mass ratio of the oil phase to the wate...

Embodiment 3

[0056] Add 300g of deionized water, 3.0g of polyvinyl alcohol, and 0.30g of sodium lauryl sulfate into a 400mL beaker (the mass ratio of ionized water, sodium lauryl sulfate, and polyvinyl alcohol is 100:0.1:1), Heat to 95°C to completely dissolve the polyvinyl alcohol and sodium lauryl sulfate to obtain an aqueous phase, which is transferred to a water bath to keep the temperature down to 55°C.

[0057] Weigh 3.25g of maleic rosin ethylene glycol acrylate, dissolve it in 80.0g of ethyl acetate, and use ultrasonic waves to promote dissolution. After the cross-linking agent is completely dissolved, add 1.55g of α-methacrylic acid and 3.0g of isooctane in sequence , 1.0g of azobisisobutyronitrile (the mass ratio of functional monomer, crosslinking agent, solvent, porogen, and initiator is 1.55:3.25:80:3:1), ultrasonically oscillated for 10min, dispersed evenly, and obtained oil Mutually.

[0058] Add the prepared oil phase to the water phase (the mass ratio of the oil phase to ...

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Abstract

The invention discloses a method for separating camptothecin and 10-hydroxycamptothecin by the adoption of rosin-based macromolecules. According to the method, alpha-methacrylic acid (or methyl methacrylate) is used as a monomer, maleated rosin-[(2-acryloyloxy) ethyl] ester is used as a cross-linking agent, and an micro-suspension free radical polymerization method is adopted to prepare rosin-based macromolecule microspheres, wherein the microspheres are a spherical porous material, the article size distribution of the rosin-based macromolecule microspheres is 3-10 microns, the average pore size of the rosin-based macromolecule microspheres is 10-15 nm, the specific surface area of the rosin-based macromolecule microspheres is 90-120 m<2> / g, and the acid value of the rosin-based macromolecule microspheres is 50-150 mgKOH / g; wet column packing is conducted on the rosin-based macromolecule microspheres by the adoption of a column packing machine, so that a chromatographic column is prepared; HPLC separation is conducted on the camptothecin and the 10-hydroxycamptothecin, wherein the detecting wave length is 230-290 nm, the temperature is 30+ / -10 DEG C, the flow speed is 0.3-1.0 mL / min, and the separation degree of the camptothecin and the 10-hydroxycamptothecin is 1.80-2.15. By the adoption of the method for separating the camptothecin and the 10-hydroxycamptothecin by the adoption of the rosin-based macromolecules, a high separation degree of the camptothecin and the 10-hydroxycamptothecin is achieved, the selectivity is high, the method is high in sensitivity, easy to operate, rapid and efficient, and no secondary pollution to medicine, health care products and food is caused.

Description

technical field [0001] The invention belongs to the field of high-performance liquid chromatography, in particular to a method for efficiently separating camptothecin and 10-hydroxycamptothecin by using a rosin-based polymer chromatographic column. Background technique [0002] Camptothecin, chemical structural formula: [0003] [0004] Camptothecin is an indole alkaloid contained in camptothecin, which has significant anticancer activity and is the third largest natural anticancer drug in plant resources. Camptothecin has good effects on gastrointestinal tract and head and neck cancer. It exerts cytotoxicity by inhibiting topoisomerase I; its structure is similar to 10-hydroxycamptothecin, but its pharmacological effects are different. [0005] 10-Hydroxycamptothecin, chemical structural formula: [0006] [0007] 10-Hydroxycamptothecin is an indole alkaloid with less content in camptothecin, and it can also be synthesized by camptothecin. It not only has higher p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D491/22C08F289/00C08F220/06C08F220/14C08F2/20B01D15/08
CPCB01D15/08C07D491/22C08F2/20C08F289/00
Inventor 王婷雷福厚王振李鹏飞宋小妹覃丽婷黄春霞
Owner GUANGXI UNIV FOR NATITIES
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