多模板分子印迹聚合物磁性固相萃取-高效液相色谱法测定环境水样中四环素类抗生素  

Determination of Tetracyclines in Environmental Water Samples by High Performance Liquid Chromatography with Multi-template Molecularly Imprinted Polymer Magnetic Solid Phase Extraction

作　　者：曾国龙 马晓国[1] 樊银明 ZENG Guo-long;MA Xiao-guo;FAN Yin-ming(School of Environmental Science and Engineering,Guangdong University of Technology,Guangzhou 510000,China)

机构地区：[1]广东工业大学环境科学与工程学院,广东广州510000

出　　处：《分析测试学报》2020年第6期749-755,共7页Journal of Instrumental Analysis

基　　金：广州市科技计划项目(201803030040)。

摘　　要：以介孔硅磁性氧化石墨烯为载体,四环素、土霉素、金霉素、强力霉素共同作为模板,N-[3-(三甲氧基甲硅烷基)丙基]乙二胺(KH-792)和苯胺甲基三乙氧基硅烷(KH-42)为功能单体,通过溶胶-凝胶法制备了四环素类抗生素多模板分子印迹聚合物。以扫描电镜(SEM)、红外光谱(IR)及振动样品磁强计(VSM)对聚合物进行表征。将所制备的多模板分子印迹聚合物作为吸附剂应用于磁性固相萃取,结合高效液相色谱法,建立了水样中四环素、土霉素、金霉素及强力霉素测定的新方法。该方法对4种四环素类抗生素的线性范围为5~50μg/L,检出限为0.67~0.95μg/L,定量下限为2.13~3.50μg/L。实际样品的加标回收率为82.7%~103%,相对标准偏差(RSD)为1.0%~8.8%。方法可用于实际环境水样中4种四环素类抗生素的同时检测。A novel high performance liquid chromatography(HPLC) with magnetic solid phase extraction(MSPE) based on multi-template molecularly imprinted polymer(MIP) was developed for the detection of tetracyclines in environmental water samples.The multi-template MIP was prepared by sol-gel method,with mesoporous silicon magnetic graphene oxide as carrier,tetracycline,oxytetracycline,chlortetracycline and doxycycline as templates,and N-[3-(trimethoxysilyl)propyl]ethylenedi amine(KH-792) and anilinomethyl triethoxysilane(KH-42) as functional monomers,which was characterized by field emission scanning electron microscopy(SEM),infrared spectroscopy(IR) and vibrating sample magnetometry(VSM).The method was applied in the detection of tetracycline,oxytetracycline,chlortetracycline and doxycycline in water samples.Results showed that the calibration curves for 4 tetracyclines were linear in the range of 5-50 μg/L,with their detection limits and quantitation limits of 0.67-0.95 μg/L and 2.13-3.50 μg/L,respectively.The spiked recoveries ranged from 82.7% to 103% with relative standard deviations(RSD) of 1.0%-8.8%.The proposed method could be used for the simultaneous and selective detection of these four tetracyclines in real environmental water samples.

关 键 词：四环素类抗生素 多模板分子印迹聚合物 磁性固相萃取 高效液相色谱(HPLC) 

分 类 号：O657.72[理学—分析化学] R978.1[理学—化学]