大粒径磺酸基固相萃取填料的制备及其对弱碱性非法添加物的吸附性能评价

Preparation of large particle size sulfonic acid group solid phase extraction packing and the evaluation of its adsorption performance for weakly alkaline illegal additives

以聚苯乙烯微球为基材,制得磺酸基阳离子固相萃取填料,对其粒径、担载量进行优化,应用于3种β-受体激动剂和三聚氰胺的浓缩富集,并结合响应面分析得到检测不同物质时所需填料的最佳担载量。与传统浓硫酸法相比,氯磺酸法制备填料时,反应温度低、试剂用量少、反应时间短,成本大大降低,同时通过控制氯磺酸用量,可以定量化制备特定担载量的磺酸基阳离子填料,应用于不同食品基质;在满足检测要求的条件下,前处理过程中使用大粒径(170μm)填料,不易堵塞小柱,能够有效缩短固相萃取时间。该研究制备的粒径170μm、担载量1.39 mmol/g的填料对3种β-受体激动剂的回收率为88%~97%,相对标准偏差为5.23%~8.99%;粒径170μm、担载量3.05 mmol/g的填料对三聚氰胺的回收率为88%,相对标准偏差为2.97%。填料满足痕量检测的要求,可用于食品中β-受体激动剂和三聚氰胺的富集吸附。

Polystyrene(PS)microspheres was used to prepare the sulfonic acid group cationic solid phase extraction packing,and then the particle size and loading amount were optimized.The solid phase extraction column could be successfully applied to the detection of threeβ-receptor agonists and melamine.At the same time,combined with response surface analysis to obtain the optimal loading of fillers required for detection of different substances.The results showed that the recoveries of the threeβ-agonists with a particle size of 170 mm and a loading amount of 0.72 mmol/g were 88%-97%,and the relative standard deviation was 5.23%-8.99%.The recovery rate of melamine with a loading of 3.05 mmol/g filler was 88%,and the relative standard deviation was 2.97%.The filler meets the requirements of trace detection and reaches the international level.Under the premise of obtaining the same performance,the large particle size(170 mm)sulfonic acid-based cationic solid phase extraction packing can not only reduce the solid phase extraction time,but also no clogging.Besides,this method not only has low reaction temperature,less reagent dosage and short reaction time,but also greatly reduces the cost.It can quantitatively prepare fillers with specific loadings and apply them to different complex food matrices.