Method for efficient separation of camptothecin and 10-hydroxycamptothecin by core-shell SiO2@rosin-based polymer chromatographic column

A hydroxycamptothecin, core-shell type technology is applied in the field of high performance liquid chromatography, and can solve the problems of cumbersome preparation process of stationary phase fillers, low separation between 10-hydroxycamptothecin and camptothecin, and rosin-based polymer chromatography. The problem of low number of theoretical plates in the column can achieve the effect of good separation performance, rich pore structure and rich surface functional groups.

Active Publication Date: 2019-04-19
GUANGXI UNIV FOR NATITIES +1
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

However, the preparation process of its stationary phase filler (rosin-based polymer microspheres) is cumbersome and the theoretical plate number of the rosin-based polymer chromatographic column prepared by it is low, which is difficult for the separation of 10-hydroxycamptothecin and camptothecin. Therefore, it is necessary to explore a more efficient method for separating camptothecin and 10-hydroxycamptothecin

Method used

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  • Method for efficient separation of camptothecin and 10-hydroxycamptothecin by core-shell SiO2@rosin-based polymer chromatographic column
  • Method for efficient separation of camptothecin and 10-hydroxycamptothecin by core-shell SiO2@rosin-based polymer chromatographic column
  • Method for efficient separation of camptothecin and 10-hydroxycamptothecin by core-shell SiO2@rosin-based polymer chromatographic column

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preparation Embodiment 1

[0044] 2.0g of methacrylic acid, 2.0g of maleopimaric acid ethylene glycol acrylate and 0.2g of azobisisobutyronitrile were fully mixed, evenly coated on the surface of 400g of silica gel, and then placed in 1000mL of 1% mass fraction of ten Carry out free radical polymerization reaction in aqueous solution of dialkyl sodium sulfate for 8 hours, then perform Soxhlet extraction of the product with absolute ethanol, and then vacuum-dry to obtain core-shell SiO 2 @ Rosin-based polymer microspheres.

[0045] After detection and analysis, the core-shell type SiO obtained in this embodiment 2 The particle size distribution of @rosin-based polymer microspheres is concentrated in the range of 2-10μm, the average pore size is 0.50nm, and the specific surface area is 350m 2 / g.

preparation Embodiment 2

[0047] After fully mixing 7.5g of methacrylic acid, 1.5g of propylene pimaric acid ethylene glycol acrylate and 2.25g of azobisisoheptanonitrile, they are evenly coated on the surface of 225g of silica gel, and then placed in 100mL of 5% dodecyl The free radical polymerization reaction was carried out in an aqueous solution of sodium alkyl sulfate for 9 hours, and then the product was subjected to Soxhlet extraction with absolute ethanol, and then vacuum-dried to obtain the core-shell SiO 2 @ Rosin-based polymer microspheres.

[0048] After detection and analysis, the core-shell type SiO obtained in this embodiment 2 The particle size distribution of @rosin-based polymer microspheres is concentrated around 12-18μm, the average pore size is 3.79nm, and the specific surface area is 247m 2 / g.

preparation Embodiment 3

[0050] After fully mixing 0.5g methyl methacrylate, 10g maleopimaric acid ethylene glycol acrylate and 14mg dibenzoyl peroxide, evenly apply it to the surface of 10.5g silica gel, and then place it in 100mL of 15% mass fraction Carry out free radical polymerization reaction in aqueous solution of sodium lauryl sulfate for 10 h, then perform Soxhlet extraction of the product with absolute ethanol, and then vacuum dry to obtain core-shell SiO 2 @ Rosin-based polymer microspheres.

[0051] After detection and analysis, the core-shell type SiO obtained in this embodiment 2 The particle size distribution of @rosin-based polymer microspheres is concentrated around 25-30μm, with an average pore size of 6.01nm and a specific surface area of ​​312m 2 / g.

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Abstract

The invention discloses a method for efficient separation of camptothecin and 10-hydroxycamptothecin by a core-shell SiO2@rosin-based polymer chromatographic column. The method includes: taking methacrylic acid or methyl methacrylate as the monomer, adopting maleopimaric acid ethylene glycol acrylate or acrylpimaric acid ethylene glycol acrylate as the cross-linking agent, fully mixing the substances with a free radical initiator, then coating a silica gel surface with the mixture, and then carrying out free radical polymerization reaction to obtain core-shell SiO2@rosin-based polymer microspheres, which have a particle size distribution of 2-50microm, a pore size distribution of 0.5-15nm and a specific surface area of 150-350m<2>/g; subjecting the core-shell SiO2@rosin-based polymer microspheres to wet packing to prepare a chromatographic column, using the prepared chromatographic column for HPLC separation on camptothecin and 10-hydroxycamptothecin, and setting the detection wavelength at 254nm, the temperature at 30+/-10DEG C and the flow rate at 0.3-1.0mL/min, thus achieving a camptothecin and 10-hydroxycamptothecin separation degree of 2.45-3.47. The method provided by the invention has high separation degree and selectivity on camptothecin and 10-hydroxycamptothecin, and also has the advantages of high sensitivity, simple operation, high speed and efficiency, and environmental friendliness.

Description

technical field [0001] The invention belongs to the field of high performance liquid chromatography, and in particular relates to an application of core-shell type SiO 2 A method for efficiently separating camptothecin and 10-hydroxycamptothecin on a rosin-based polymer chromatographic column. Background technique [0002] Camptothecin, the chemical structural formula is: [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, the chemical structure is: [0006] [0007] 10-Hydroxycamptothecin is an indole alkaloid with less content in camptothecin, and it can also be sy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D491/22
CPCC07D491/22
Inventor 雷福厚孙耀李鹏飞王婷姚兴东覃丽婷程格格鄂羽羽杨建林
Owner GUANGXI UNIV FOR NATITIES
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