摘要
釆用分子印迹固相萃取结合高效液相色谱法,建立检测水产品中5种丁香酚类麻醉剂残留的方法。分别使用丁香酚、甲基丙烯酸、乙二醇二甲基丙烯酸酯作为模板分子、功能单体和交联剂,采用本体聚合法制备合成分子印迹聚合物并制成萃取柱。通过响应面分析法得出模板分子、功能单体、交联剂的最佳比例14.5523.21;样品溶剂选择甲醇能使5种丁香酚类化合物回收率达到90%;洗脱剂选择91的甲醇乙酸溶液能够使5种丁香酚类化合物回收率达90%以上;该方法的线性范围均为0.05-10μg/mL,相关系数为0.999 83-0.999 97,具有较好的线性关系;5种丁香酚类麻醉剂的定量限为0.05 mg/kg。该方法对样品的回收率为82.04%-99.29%,RSD为0.06%-3.96%。所建立的方法具有简单便于操作、准确快速、操作可行性高、有机溶剂耗量少等特点,可用于水产品中5种丁香酚类麻醉剂残留的测定。
A new method of molecularly imprinted solid phase extraction （ MISPE ） combined with high performance liquid chromatography （HPLC） was developed for detecting five kinds of clove phenol anesthetic in aquatic product. Using eugenol as template molecule, methacrylic acid as functional monomer, ethylene glycol dimethacrylate as cross linking agent, molecularly imprinted polymers were synthesized by bulk polymerization and made into extraction column. Through the response surface analysis template molecule and functional monomer, crosslinking agent the best proportion was 1 ： 4. 55 ： 23. 21, and the recovery rate of these com- pounds reached 90~ by using methanol as solvent and acetic acid solution as eluent. The results showed that linear response data were obtained in the concentration range of 0.05- 10μg/mL for the five kinds of clove phenol anesthetic with correlation coefficients from 0.999 83 to 0.999 97, and the limits of quantitative were 0.05 mg/kg. The method of sample recovery rate was 82.04%-99.29% with the relative standard deviations ranging from 0.06%-3.96%. The new established method was found simple and fast, accurate and feasible, and this could be successfully applied for the determination of five kinds of clove phenol anesthetic in aquatic product and their residue with low solvent consumption.
出处
《食品与机械》
CSCD
北大核心
2016年第11期39-44,67,共7页
Food and Machinery
基金
广东省科技计划项目(编号:2014A020208121)
关键词
分子印迹聚合物
分子印迹固相萃取
高效液相色谱法
水产品
丁香酚类麻醉剂
Molecularly imprinted polymer
molecularly imprinted solid phase extraction （M1SPE）
high performance liquid chromatography （HPLC）
aquatic product
clove phenol anesthetic
