首页|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

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

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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.
Preparation of Hydrophilic-Lipophilic Balance Polymer Microspheres and Its Application in Veterinary Drug Residue Analysis
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 adsorption-desorption 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 home-made 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 home-made 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.

hydrophilic-lipophilic balance polymer microspheressuspension polymerizationsolid-phase extractionveterinary drug residuesliquid chromatography-tandem mass spectrometry

何冲、李俭、李媛、王博宇、刘家玮、吴坤

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陕西省产品质量监督检验研究院(西安 710048)

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)

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

2024

食品工业
上海市食品工业研究所

食品工业

影响因子:0.47
ISSN:1004-471X
年,卷(期):2024.45(11)