A kind of capillary monolithic column of nucleoside polymer matrix and its preparation method and application
A technology of capillary monolithic columns and nucleoside polymers, applied in separation methods, chemical instruments and methods, and other chemical processes, can solve the problems of lack and difficulty in preparing capillary monolithic columns, and achieve the effect of good permeability
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Embodiment 1
[0025] 1. Column pretreatment
[0026] The inner wall of the capillary was rinsed with acetone for 30 minutes, water for 1 hour, sodium hydroxide for 12 hours, water for 2 hours, hydrochloric acid for 3 hours, water for 2 hours, methanol for 30 minutes, and finally nitrogen to dry;
[0027] 2. Silanization
[0028] A mixture of anhydrous methanol and methacryloxypropyltrimethoxysilane (γ-MAPS) with a volume ratio of 1:1 was injected into the pretreated capillary, reacted at 45 °C for 12 h, and then rinsed with methanol for 30 min , blow dry under nitrogen at 60°C;
[0029] 3. In-column synthesis
[0030] Accurately weigh out 60 mg of 3'-azido-3'-deoxythymidine, 31 μL of propargyl methacrylate, 60 mg of pentaerythritol triacrylate, 175 μL of dimethyl sulfoxide, 192 μL of dodecanol, and azobisisobutylene 1.5 mg of nitrile and 0.2 mg of cuprous iodide were placed in a centrifuge tube, sonicated at room temperature to make them evenly mixed, and nitrogen blown to make a prepoly...
Embodiment 2
[0034] In micro-column liquid chromatography (μHPLC) mode, 5% acetonitrile aqueous solution was used as mobile phase A, and 5% aqueous acetonitrile solution was used as mobile phase B; chromatographic conditions: 100% B; the pump flow rate was 0.02 mL / min; the detection wavelength was 214 nm; a mixture of toluene, thiourea, formamide, and N,N-dimethylformamide (100 ppm each) achieves highly efficient and selective nucleoside polymer-based capillary monolithic columns prepared in Example 1 above. separation, the chromatographic separation diagram is as follows image 3 As shown, the peaks in the chromatogram are 1: toluene, 2: N,N-dimethylformamide, 3: formamide, and 4: thiourea.
Embodiment 3
[0036] In micro-column liquid chromatography (μHPLC) mode, 5% acetonitrile aqueous solution was used as mobile phase A, and 5% water acetonitrile solution was used as mobile phase B; chromatographic conditions: 45% B; the pump flow rate was 0.02 mL / min; the detection wavelength was 214nm; the mixture of benzene, toluene, ethylbenzene, propylbenzene, and butylbenzene (100ppm each) can achieve efficient and selective separation on the capillary monolithic column of the nucleoside polymer matrix prepared in Example 1 above, and its chromatographic separation turu Figure 4 As shown, the peaks in the chromatogram are 1: benzene, 2: toluene, 3: ethylbenzene, 4: propylbenzene, and 5: butylbenzene.
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