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| Preparation and Application of Dehydroabietic Acid Glycidyl Methacrylate Ester-bonded Silica Stationary Phase |
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| DOI： |
| KeyWord:dehydroabietic acid bonded stationary phase retention mechanism paclitaxel |
| Author | Institution |
| ZENG Lei，TANG Xiao-song，SHI Bo-an，LEI Fu-hou |
1. Guangxi Collaborative Innovation Center for Chemistry and Engineering of Forest Products，Guangxi Key Laboratory of Chemistry and Engineering of Forest Products，Key Laboratory of Chemistry and Engineering of Forest Products of State Ethnic Affairs Commission，School of Chemistry and Chemical Engineering， Guangxi Minzu University，Nanning ，China; 2. School of Chemical and Environmental Engineering，Hubei Minzu University，Enshi ，China |
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| Abstract: |
| A dehydroabietic acid glycidyl methacrylate ester（DAGME）-bonded silica stationary phase（Sil－DAGME） was fabricated in this paper．The DAGME was firstly prepared using dehydroabietic acid and glycidyl methacrylate via a ring-opening addition reaction，and then grafted onto the surface of a thiol-functionalized spherical silica by click reaction to obtain the Sil－DAGME．The successful immobilization of DAGME on the silica was confirmed through series of characterizations including Fourier-transform infrared spectroscopy（FT－IR），thermal gravimetric analysis（TGA） and elemental analysis（EA）．The chromatographic performance and retention mechanisms of Sil－DAGME were validated using a variety of compounds including alkylbenzenes，Tanaka standard test mixtures，polycyclic aromatic hydrocarbons，phenols and flavonoids．Meanwhile，the Sil－DAGME exhibits multiple interactions，including hydrophobic，π－π and hydrogen bonding interaction between the stationary phase and the analytes during the separation process due to the co-existing of benzene ring，carbonyl group，hydroxyl group and hydrophobic rigid tricyclic hydrophenanthrene skeleton in the DAGME on the silica surface．Based on synergistic action of multiple retention mechanisms，the probe molecules metioned above achieved ideal resolution and flexible selectivity in separation．In addition，the Sil－DAGME not only exhibited good stability，repeatability and reproducibility with the run-to-run relative standard deviations（RSDs） of 0.050%－0.19%（n = 10），the day-to-day RSDs of 0.25%－1.0%（n = 7），and the column-to-column RSDs of 0.78%－2.1%（n = 3） for the retention time，but also showed an excellent separation ability for Yew tree bark extract．In short，the application of dehydroabietic acid in chromatographic separation materials not only provided a new approach for the separation and detection of paclitaxel，but also presented a reference for the design stationary phase using natural product rosin as functional ligand. |
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