核壳型松香基高分子键合硅胶液相色谱固定相高效分离紫杉醇

doi:10.3969/j.issn.0253-2417.2023.01.004

Abstract

Abstract:

A rosin-based core-shell polymer bonded silica(RP@SiO₂) stationary phase was prepared by the radical polymerization of fumaropimaric acid tri(β-acryloxyl ethyl) ester(FATE) onto alkylated silica(TPM-SiO₂). The RP@SiO₂ stationary phase was characterized and evaluated, the separation performance and mechanism of RP@SiO₂ column for paclitaxel(PTX) and its analogs were discussed, and it was used for the separation and purification of PTX from crude yew-bark extract. The results showed that FATE was successfully bonded to the surface of silica, the core-shell structure material was successfully prepared, and the average particle size of RP@SiO₂ was about 5 μm. The RP@SiO₂ column was a typical reversed-phase column similar to C18 column, showing excellent chromatographic performance, satisfactory performance reproducibility, and typical reversed-phase chromatographic behavior. The RP@SiO₂ column was used to separate paclitaxel analogs, and the separation degree of continuous elution samples was more than 6.6. Stoichiometric displacement theory for retention(SDT-R) and van't Hoff thermodynamic analysis showed that hydrophobic interactions determined the analyte retention, and the separation of paclitaxel analogs on RP@SiO₂ column was an exothermic process driven by enthalpy. Furthermore, SDT-R could be used to explain its retention mechanism. The RP@SiO₂ column was employed to separate and purify paclitaxel from crude yew-bark extract, increasing paclitaxel purity from 6% to 81%.

Key words: rosin-based stationary phase, HPLC, retention mechanism, paclitaxel

CLC Number:

TQ35
O658

Hao LI, Wenbo XIE, Lei ZENG, Liuyu YI, Wen LI, Fuhou LEI. Highly Effective Separation of Paclitaxel by Using Core-shell Rosin-based Polymer Bonded Silica as Liquid Chromatography Stationary Phase[J]. Chemistry and Industry of Forest Products, 2023, 43(1): 34-42.

Figures/Tables 9

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Table 1

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Table 2

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References 21

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分析物analyte	lgI	Z	R²
10-DAB	1.85±0.15	2.40±0.17	0.977
BCT	2.25±0.13	2.50±0.14	0.987
10-DAT	3.94±0.06	4.07±0.07	0.998
CEP	4.18±0.07	4.19±0.07	0.998
PTX	4.61±0.05	4.57±0.06	0.999

分析物 analyte	回归方程 regression equation	R²	ΔH/ (kJ·mol^-1)	ΔS/ (J·mol^-1·K^-1)	ΔΔH/ (kJ·mol^-1)	ΔΔS/ (J·mol^-1·K^-1)
10-DAB	lnk=-0.682 4+153.66/T	0.947	-1.278	-5.673	-0.993	2.833
BCT	lnk=-0.448 3+306.22/T	0.991	-2.546	-3.727	-1.606	4.194
10-DAT	lnk=-0.046 73+531.58/T	0.991	-4.420	-0.389	-0.916	2.462
CEP	lnk=0.205+556.58/T	0.995	-4.627	1.704	-0.702	0.317
PTX	lnk=0.239 9+642.01/T	0.989	-5.338	1.995

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Highly Effective Separation of Paclitaxel by Using Core-shell Rosin-based Polymer Bonded Silica as Liquid Chromatography Stationary Phase

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