分子印迹固相萃取-高效液相色谱法检测奶粉中3种β-兴奋剂  

Detection of three kinds of β-Agonists in milk powder by molecularly imprinted solidphaseextraction-highperfrmance liquid chromatography

作　　者：魏盘 王建[1] 石雨 祁迎春[1] 任景俞 黄华[1] 牛志睿[1] 孙召 WEI Pan;WANG Jian;SHI Yu;QI Yingchun;REN Jingyu;HUANG Hua;NIU Zhirui;SUN Zhao(Key Laboratory of Environmental Testing and Restoration,School of Petroleum Engineering and Environmental Engineering,Yan'an University,Yan'an 716000,China)

机构地区：[1]延安市环境检测与修复重点实验室,延安大学石油工程与环境工程学院,延安716000

出　　处：《分析试验室》2024年第6期793-798,共6页Chinese Journal of Analysis Laboratory

基　　金：国家自然科学基金项目(21864025);陕西省自然科学基础研究计划项目(2018JM2052);陕西省教育厅科学研究计划项目(18JK0868);大学生创新创业训练计划项目(S201910719045)资助。

摘　　要：以β-兴奋剂3-甲氧酪胺(3-MT)、多巴胺(DA)和去氧肾上腺素(PE)为模板,采用沉淀聚合法,分别制备了3种单模板分子印迹聚合物(SMIP)和3种混合模板分印迹聚合物(MMIP),并在水和乙醇中对其吸附和分离性能进行了评价。结果表明,以3-MT为模板的SMIP1在乙醇中对上述3种β-兴奋剂具有最佳选择性,25 min可达吸附平衡。在对3-MT的初始浓度为0.03 mmol/L时,印迹因子(IF)最大,为2.12。SMIP1对3-MT,DA和PE的吸附量随吸附初始浓度增加而增加,在3 mmol/L时分别达到41.26,39.83和40.47μmol/g。以SMIP1为吸附剂从奶粉中同时高选择性固相萃取3-MT,DA和PE,在上样浓度为0.01,0.02和0.03 mmol/L时,高效液相色谱法(HPLC)检测的回收率分别为98%~100%,92.5%~96%和90.3%~94%,相对标准差(RSD)分别为1.9%~5.1%,2.0%~4.0%和2.1%~4.2%。该方法适用于奶粉中3-MT的定量分析以及DA和PE的定性检测。In this study,three single-template molecular imprinted polymers(SMIP)and three mixed templatemolecular imprinted polymers(MMIP)were prepared by precipitation polymerization using 3-methoxytyine(3-MT),dopamine(DA)and phenylephrine(PE)as the templates,and their adsorption and separation performance were evaluated in water and ethanol.The performance tests showed that the adsorption capacity of SMIP1 with 3-MT as template had the best selectivity for the above threeβ-Agonists in ethanol,and the adsorption equilibrium can be reached at 25 min.At an initial concentration of 0.03 mmol/L,the imprinting factor(IF)reached the highest value of 2.12.The adsorption capacity of SMIP1 for 3-MT,DA and PE increased with the initial concentration,and the adsorption capacity were determined to be 41.26,39.83 and 40.47μmol/g at an initial concentration of 3 mmol/L.The selective simultaneous extraction of 3-MT,DA and PE from milk powder were achieved by employing this SMIP1 as a solid phase extraction adsorbent.At the spiked concentrations of 0.01,0.02 and 0.03 mmol/L,the mean recoveries of 3-MT,DA and PE,as detected by high performance liquid chromatography(HPLC)method,ranged from 98%to 100%,92.5%to 96%,and 90.3%to 94%,respectively.The relative standard deviations(RSD)ranged from 1.9%to 5.1%,2.0%to 4.0%and 2.1%to 4.2%,respectively.This method is suitable for quantitative analysis of 3-MT and qualitative detection of DA and PE in milk powder.

关 键 词：兴奋剂 分子印迹聚合物 固相萃取 奶粉 

分 类 号：O657[理学—分析化学]