Preparation of a polyacrylamide-wrapped composite silica gel and its application as a chromatographic packing
A technology of polyacrylamide and silica gel, applied in the field of high-performance liquid chromatography separation and analysis, which can solve the problems of expensive chromatographic columns and complicated preparation process, and achieve the effects of excellent separation effect, green synthesis process and reduced laboratory cost
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Embodiment 1
[0023] PAM@SiO 2 The preparation of the filler includes the following steps:
[0024] (1) Silica gel activation: take 8 g of silica gel, heat under reflux with 6 mol / L hydrochloric acid for 4 h, wash with water until neutral, and vacuum dry at 70 °C for 6 h for use;
[0025] (2) Preparation of polyacrylamide solution: take 0.2 g of polyacrylamide solid particles with a molecular weight of 10 million, add it to 1000 mL of distilled water, and stir magnetically for 24 h to dissolve it uniformly;
[0026] (3) Silica gel surface modification and curing: Take 5 g of activated silica gel, add it to 150 mL of polyacrylamide solution, ultrasonically treat it for 10 min, and then magnetically stir at 70 °C until the solution evaporates to dryness. Wash once with aqueous solution. The composite microspheres prepared above were dried under vacuum at 70 °C for 8 h to cure the polyacrylamide molecules coated on the surface of the silica gel;
[0027] (5) Polyacrylamide-wrapped composite...
Embodiment 2
[0028] Example 2. Chromatographic separation of ribose
[0029] PAM@SiO 2 Preparation of chromatographic column: The PAM@SiO prepared in Example 1 was prepared by high pressure homogenization method. 2 The chromatographic packing is packed into a 150×4.6mm stainless steel liquid chromatographic column, which is used for the separation and analysis of sugar compounds. During the filling process, the dispersion liquid was carbon tetrachloride, the displacement liquid was n-hexane, and the pressure was 40 MPa.
[0030] Chromatographic separation of ribose: The chromatographic analysis conditions are as follows: mobile phase is 90% acetonitrile aqueous solution; flow rate is 1.0mL / min; evaporative light scattering detector, gas flow rate is 4 L / min, temperature is 115℃; injection volume is 20µL .
[0031] The liquid chromatogram of ribose see figure 2 . Under the above chromatographic analysis conditions, the retention time of ribose was 4.3 min, and the column efficiency wa...
Embodiment 3
[0032] Example 3. Chromatographic separation of arabinose
[0033] PAM@SiO 2 Preparation of chromatographic column: The PAM@SiO prepared in Example 1 was prepared by high pressure homogenization method. 2 The chromatographic packing is packed into a 150×4.6mm stainless steel liquid chromatographic column, which is used for the separation and analysis of sugar compounds. During the filling process, the dispersion liquid was carbon tetrachloride, the displacement liquid was n-hexane, and the pressure was 40 MPa.
[0034] Chromatographic separation of arabinose: The chromatographic analysis conditions are as follows: mobile phase is 90% acetonitrile aqueous solution; flow rate is 1.0mL / min; evaporative light scattering detector, gas flow rate is 4 L / min, temperature is 115℃; injection volume is 20µL.
[0035] The liquid chromatogram of arabinose see image 3 . The retention time of arabinose was 6.4 min, and the column efficiency was about 60000 / m.
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