虚拟模板分子印迹材料固相萃取磺胺类抗生素  

Solid-phase Extraction of Sulfonamides Antibiotics by Using Dummy Template Based Molecularly Imprinted Materials

作　　者：王艺晓 孙宏宵 王莉燕 纪灵[5] 孙大妮 刘惠涛[4] 宋志花 李金花[1,6] WANG Yi-xiao;SUN Hong-xiao;WANG Li-yan;JI Ling;SUN Da-ni;LIU Hui-tao;SONG Zhi-hua;LI Jin-hua(Shandong Key Laboratory of Coastal Environmental Processes,CAS Key Laboratory of Coastal Environmental Processes and Ecological Remediation,Shandong Research Center for Coastal Environmental Engineering and Technology,Yantai Institute of Coastal Zone Research,Chinese Academy of Sciences,Yantai 264003,China;School of Environmental and Material Engineering,Yantai University,Yantai 264005,China;Collaborative Innovation Center of Advanced Drug Delivery System and Biotech Drugs in Universities of Shandong,Key Laboratory of Molecular Pharmacology and Drug Evaluation(Yantai University),Ministry of Education,School of Pharmacy,Yantai University,Yantai 264005,China;College of Chemistry and Chemical Engineering,Yantai University,Yantai 264005,China;Yantai Oceanic Environmental Monitoring Central Station,State Oceanic Administration,Yantai 264006,China;University of Chinese Academy of Sciences,Beijing 100049,China)

机构地区：[1]中国科学院烟台海岸带研究所,山东省海岸带环境工程技术研究中心,中国科学院海岸带环境过程与生态修复重点实验室,山东省海岸带环境过程重点实验室,山东烟台264003 [2]烟台大学环境与材料工程学院,山东烟台264005 [3]烟台大学药学院,分子药理和药物评价教育部重点实验室,新型制剂与生物技术药物研究山东省高校协同创新中心,山东烟台264005 [4]烟台大学化学化工学院,山东烟台264005 [5]国家海洋局烟台海洋环境监测中心站,山东烟台264006 [6]中国科学院大学,北京100049

出　　处：《化学试剂》2022年第9期1314-1324,共11页Chemical Reagents

基　　金：国家自然科学基金资助项目(21876199,22176210);山东省自然科学基金资助项目(ZR2020KC032);烟台市科技创新发展计划项目(2020MSGY112,2020MSGY077)。

摘　　要：以磺胺苯(SZ)为虚拟模板,一步沉淀聚合制备虚拟模板分子印迹聚合物(DMIPs)材料,用于同时分散固相萃取(DSPE)水样中4种磺胺类(SAs)抗生素,结合HPLC-UV进行测定。对DMIPs进行表征与吸附性能评价,其对4种SAs的最大吸附量为21.97~30.24 mg/g,印迹因子均大于2.1。优化DMIPs用量、萃取时间、样品溶液pH等,确定最佳DSPE和HPLC条件。在湖水、海水、自来水中评价方法的分析性能,得到3种水样中的线性范围为1~200μg/L、检出限0.27~0.64μg/L和定量限0.96~2.14μg/L。基质效应(ME%≤6%)结果表明DMIPs-DSPE有效消除了复杂基质干扰,提高了检测准确度。4种SAs在3种水样中的回收率为93.8%~102.6%,相对标准偏差(RSD)为2.6%~7.0%。该DMIPs-DSPE-HPLC-UV法简单快速、灵敏准确,适于复杂样品中痕量SAs多残留分析。Dummy template molecularly imprinted polymers(DMIPs)were prepared by one-step precipitation polymerization using sulfameobenzene(SZ)as a dummy template,and applied for the simultaneous dispersion of four typical SAs in solid-phase extraction(DSPE),followed by high performance liquid chromatography-UV(HPLC-UV)determination.The DMIPs was characterized by several techniques,such as SEM and FT-IR,and its static/dynamic adsorption and selectivity were all evaluated by using adsorption models.The maximum adsorption capacities of DMIPs towards the four SAs including sulfamonomethoxine(SMM),sulfachloropyridazine(SFZ),sulfamethoxazole(SMX)and sulfadimethoxine(SDM)were 21.97~30.24 mg/g,and the imprinting factors were all greater than 2.1.The factors affecting the extraction efficiency of DMIPs-DSPE,mainly including dosage of DMIPs,extraction time,pH of sample solution,volume of desorption and time of desorption were systematically optimized.Under the optimal conditions,the DMIPs-DSPE-HPLC-UV methods attained good linearity in the range of 1~200μg/L with correlation coefficients≥0.9995,and the limits of detection(LODs)were 0.27~0.64μg/L and the limits of quantification(LOQs)were 0.96~2.14μg/L in lake water,seawater and tap water samples.The precision of the method was excellent,for example,the intraday precision(relative standard deviation,RSD)of retention time and peak area of the four SAs were 0.07%~0.13%and 0.53%~1.13%,respectively,and the interday precision was 0.41%~0.88%and 0.63%~2.16%,respectively.The matrix effect(ME)of the method was investigated to be ME≤6%in the above three water samples,indicating that the developed method can effectively eliminate the interference of complex matrices.The recoveries of four SAs in lake water,seawater,tap water were 93.8%~99.8%,94.8%~100.1%and 95.6%~102.6%,respectively,with RSD of 2.6%~7.0%,2.8%~5.4%and 2.8%~5.2%.The simple,rapid,sensitive and accurate DMIPs-DSPE-HPLC-UV method proved applicable for multiresidue analysis of SAs in complicated samples.

关 键 词：磺胺类抗生素 分子印迹聚合物 虚拟模板 固相萃取 环境水样 高效液相色谱 

分 类 号：O615.4[理学—无机化学]