Polycyclic aromatic hydrocarbon adsorbent for solid phase extraction and preparation method thereof
A polycyclic aromatic hydrocarbon and adsorbent technology, applied in the field of solid phase extraction polycyclic aromatic hydrocarbon adsorbent and its preparation, can solve the problems of poor selectivity and weak force, achieve selective adsorption, improve sensitivity and selectivity, enrichment Efficient effect
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Embodiment 1
[0033] 5 g of calcium chloride desiccant was placed in 100 mL of xylene overnight. After drying the required glassware, put it into a vacuum desiccator to cool under reduced pressure and vacuum. Set up the reflow device and replace the air in the reflow device with nitrogen. Pre-dried xylene was added under nitrogen, followed by 1 g of clipped sodium. After heating and refluxing at 162 °C for 2 hours (concentrated sulfuric acid liquid sealing and refluxing), add 0.5 g of xylene ketone, after the reflux turns blue, pass nitrogen, cool down a little, and then change to a distillation device, heat to 168 °C to distill out the xylene, put it out. Put into a molecular sieve seal and store in a desiccator.
[0034] (2) Dry triethylamine
[0035] 2 g of potassium hydroxide desiccant was added to 75 mL of triethylamine and left overnight. After drying the required glassware, put it into a vacuum desiccator to cool under reduced pressure and vacuum....
Embodiment 2
[0039] Step (1) and step (2) are the same as in Example 1. The synthesis reaction is as follows:
[0040] After drying the desired reaction device, it was cooled in a vacuum desiccator. The reaction apparatus was set up, and the air in the apparatus was replaced with nitrogen. Under nitrogen, add 10 ml of the xylene solution prepared in step (1), and then add 1 g of amine-bonded silica Bond Elut NH 2 , 0.5g of 2-bromo-1,3,4,5,6,7,8-heptafluoronaphthalene, and 0.18g of triethylamine prepared in step (2), heated to 110°C, and reacted for 48h to obtain perfluoro Naphthalene bonded silica sorbent. The perfluoronaphthalene-bonded silica gel adsorbent prepared by the reaction was washed successively with 100 mL of methanol, 50 mL of dichloromethane, and 50 mL of n-hexane. After the solvent was evaporated to dryness, it was placed in a vacuum drying box and dried in vacuum at 60°C for 12 hours.
Embodiment 3
[0042] Step (1) and step (2) are the same as in Example 1. The synthesis reaction is as follows:
[0043] After drying the desired reaction device, it was cooled in a vacuum desiccator. The reaction apparatus was set up, and the air in the apparatus was replaced with nitrogen. Under nitrogen, add 10 ml of the xylene solution prepared in step (1), and then add 1 g of amine-bonded silica Bond Elut NH 2 , 1.25g of 2-bromo-1,3,4,5,6,7,8-heptafluoronaphthalene, and 0.54g of triethylamine prepared in step (2), heated to 140°C and reacted for 18h to obtain perfluoro Naphthalene bonded silica sorbent. The perfluoronaphthalene-bonded silica gel adsorbent prepared by the reaction was washed successively with 100 mL of methanol, 50 mL of dichloromethane, and 50 mL of n-hexane. After the solvent was evaporated to dryness, it was placed in a vacuum drying box and dried in vacuum at 60°C for 12 hours.
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