亲水-亲脂平衡聚合物微球的制备及其在兽药残留分析中的应用  

Preparation of Hydrophilic-Lipophilic Balance Polymer Microspheres and Its Application in Veterinary Drug Residue Analysis

作　　者：何冲 李俭 李媛 王博宇 刘家玮 吴坤 HE Chong;LI Jian;LI Yuan;WANG Boyu;LIU Jiawei;WU Kun(Shaanxi Institute of Product Quality Supervision and Inspection,Xi’an 710048;Key Laboratory of Synthetic and Natural Functional Molecule of the Ministry of Education,College of Chemistry&Materials Science,Northwest University,Xi’an 710127)

机构地区：[1]陕西省产品质量监督检验研究院,西安710048 [2]合成与天然功能分子教育部重点实验室,西北大学化学与材料科学学院,西安710127

出　　处：《食品工业》2024年第11期43-49,共7页The Food Industry

基　　金：陕西省市场监督管理局科技计划项目(项目号2022KY05)。

摘　　要：研究以二乙烯苯(DVB)和N-乙烯基吡咯烷酮(NVP)为两种聚合单体,偶氮二异丁腈(AIBN)为引发剂,甲苯和环己醇为致孔剂,羟丙基甲基纤维素(HPMC)为分散剂,通过悬浮聚合方法制备了亲水-亲脂平衡聚合物(HLB)微球,并对其进行扫描电镜分析(SEM)、X射线光电子能谱(XPS)、N2吸附-脱附等温线分析和红外表征。将研制的HLB微球作为固相萃取填料制备SPE小柱,依照GB 31658.17—2021的方法对畜禽肉中多种药物残留进行SPE净化处理,结合高效液相色谱-串联质谱仪测定。结果表明:自制HLB微球单分散性良好,粒径均匀程度高,比表面积大,孔径分布均一,表面极性和非极性基团丰富。此外,自制HLB微球填充的SPE小柱实现了畜禽肉中的33种兽药残留的同时萃取净化,测得的加标样品回收率(58.6%~102.7%)和精密度(0.1%~5.2%)均优于商品化HLB小柱(回收率46.7%~87.6%,SRSD 0.1%~8.7%),展现了自制HLB填料在兽药残留分析中的应用潜力。In this work,two polymerization monomers,i.e.,divinylbenzene(DVB)and N-vinyl-2-pyrrolidone(NVP),as well as azobisisobutyronitrile(AIBN)as the initiator,were employed to prepare hydrophilic-lipophilic balance(HLB)polymer microspheres.During the polymerization process,toluene and cyclohexanol were used as porogen agents,and hydroxypropyl methylcellulose(HPMC)was used as a dispersant.The HLB microspheres were prepared through suspension polymerization method and characterized by scanning electron microscopy(SEM),X-ray photoelectron spectroscopy(XPS),N2 adsorptiondesorption isotherm analysis,and infrared spectra.The home-made HLB microspheres were used as the packing material to prepare the solid-phase extraction(SPE)columns.Various veterinary drug residues from the livestock meat and poultry were extracted and purified by the HLB SPE columns according to GB 31658.17—2021 standard method,and high-performance liquid chromatography-tandem mass spectrometry was applied for veterinary drug analysis.The results showed that homemade HLB microspheres displayed good monodispersity,homogenous particle size,large specific surface area,uniform pore size distribution,and abundant polar and non-polar functional groups on the surface.Furthermore,the simultaneous extraction and purification of 33 kinds of veterinary drugs from livestock meat and poultry samples were achieved by using the homemade HLB microspheres packed SPE column.The recoveries ranging in 58.6%to 102.7%and the relative standard deviations(SRSD)within 0.1%to 5.2%were acquired by the home-made HLB SPE column,which were higher than those gained by the commercial HLB column(recovery:46.7%-87.6%.SRSD:0.1%-8.7%).This study clearly indicated the great potential of home-made HLB microspheres in the analysis of veterinary drug residues from complex sample matrices.

关 键 词：亲水-亲脂平衡聚合微球 悬浮聚合 固相萃取 兽药残留 液相色谱-串联质谱 

分 类 号：TS207.5[轻工技术与工程—食品科学] O657.63[轻工技术与工程—食品科学与工程]