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| Separation of Positional Isomers Using Core-shell Composite NH2－MIL－125@TPA－COF Column with High Performance Liquid Chromatography |
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| DOI： |
| KeyWord:core-shell composites ?positional isomers ?high performance liquid chromatography ?stationary phase ?separation |
| Author | Institution |
| GUO Ping，XU Na-yan，CHEN Ji-kai，ZHANG Jun-hui，WANG Bang-jin，XIE Sheng-ming，YUAN Li-ming |
Department of Chemistry and Chemical Engineering，Yunnan Normal University，Kunming ，China |
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| Abstract: |
| In this work，a core-shell MOF@COF composite，NH2－MIL－125@TPA－COF was prepared by immobilizing the COF（TPA－COF） crystals on the surface of MOF（NH2－MIL－125） particles through in-situ growth approach．The NH2－MIL－125@TPA－COF composite was characterized by powder X-ray diffraction（PXRD），Fourier transform infrared spectroscopy（FTIR） and scanning electronic microscopy（SEM）．An HPLC column（25 cm long × 2.1 mm i.d.） was successfully prepared with NH2－MIL－125@TPA－COF composite as stationary phase．Under normal-phase（n-hexane－isopropanol（9∶1，volume ratio）） and reverse-phase（methanol－water（9∶1，volume ratio）） high performance liquid chromatographic（HPLC） conditions，the separation performance of this column for a series of positional isomers was investigated．The experimental results showed that the NH2－MIL－125@TPA－COF packed column exhibited a good separation performance toward 9 positional isomers，i.e. bromonitrobenzene，nitroaniline，chlorophenol，binitrobenzene，iodoaniline，bromaniline，phenylenediamine，toluidine and chloroaniline under a low column backpressure（60－100 kPa），among which bromonitroaniline， nitroaniline and dinitrobenzene could reach the baseline separation on this column，and the highest resolution（Rs） was 9.71．Under reverse-phase HPLC condition，the column efficiencies of?o-bromonitrobenzene，m-nitroaniline and?o-chlorophenol were 18 424 plates·m－1，19 053 plates·m－1 and 12 954 plates·m－1，respectively．Under normal-phase HPLC condition，the reproducibility and stability of this column was investigated using bromonitrobenzene as the analyte．The relative standard deviations（RSD） for retention time and peak area of bromonitrobenzene for five repeated injections（50th injection，100th injection，150th injection，200th injection，and 250th injection，respectively） were 0.29% and 0.89%，respectively. The retention time，selectivity and separation performance of bromonitrobenzene on this column did not change obviously，indicating that the prepared NH2－MIL－125@TPA－COF packed column exhibited good reproducibility and stability for HPLC separation of positional isomers．The results indicated that the core-shell composite NH2－MIL－125@TPA－COF as a new type of HPLC stationary phase has a good application prospect in the separation of positional isomers. |
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