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目的建立分子印迹固相萃取与高效液相色谱联用快速测定酱油中酪胺含量的方法。方法采用本体聚合法以酪胺为模板分子,对乙烯基苯甲酸(P-VBA)为功能单体,乙二醇二甲基丙烯酸酯(EGDMA)为交联剂,制备分子印迹聚合物为填料自制固相萃取柱。对上样溶剂、流速、淋洗及洗脱溶剂等条件进行优化,采用优化的条件萃取酱油中的酪胺,高效液相色谱测定。结果固相萃取优化条件为:上样溶剂为5%乙醇水溶液,10%甲醇为淋洗液,40%乙腈为洗脱液,流速均控制在0.5 mL/min。在加标浓度为5μg/mL和10μg/mL的3种酱油所得到的平均回收率在86.95%~106.06%之间。结论本方法能快速分离酱油中酪胺,样品前处理效率高,方法灵敏度高,适用于食品中酪胺的痕量分析。
OBJECTIVE To establish a rapid method for the determination of tyramine in soy sauce by molecularly imprinted solid phase extraction and high performance liquid chromatography. Methods The bulk polymerization was carried out using tyramine as template, vinyl-p-vinyl benzoate (P-VBA) as functional monomer and ethylene glycol dimethacrylate (EGDMA) as crosslinking agent to prepare molecularly imprinted polymer Homemade solid phase extraction column. The loading solvent, flow rate, rinsing and eluting solvents and other conditions were optimized, and the tyramine in soy sauce was extracted with optimized conditions and determined by high performance liquid chromatography. Results The optimum conditions of SPE were as follows: 5% ethanol in water, 10% methanol as eluent and 40% acetonitrile as eluent, and the flow rate was controlled at 0.5 mL / min. The average recoveries of the three soy sauce spiked at concentrations of 5μg / mL and 10μg / mL ranged from 86.95% to 106.06%. Conclusion The method can rapidly separate the tyramine in soy sauce. The method has the advantages of high pretreatment efficiency, high sensitivity and is suitable for the trace analysis of tyramine in food.