摘要
目的采用聚吡咯修饰磁性纳米材料,建立环境水样中喹诺酮类药物的富集分离-超高效液相色谱-串联质谱法(UPLC-MS/MS)。方法通过化学氧化法将吡咯单体以聚合态的形式结合到Fe_3O_4磁球上形成核壳结构的功能化纳米材料,应用透射电子显微镜对材料进行表征。水样经甲酸调节pH值至4. 0,加入纳米材料,涡旋30 min,磁铁分离,2 ml 10%氨化甲醇(V/V)洗脱10 min,氮吹吹干,1 ml 0. 1%甲酸甲醇(V/V)溶解,过0. 22μm滤膜后采用HPLCMS/MS多离子反应监测(MRM)正电荷模式检测。结果 11种喹诺酮类的线性范围为5 ng/L～1 000 ng/L时,相关系数(r)均> 0. 999 0,检出限为1. 1 ng/L～3. 5 ng/L,定量限为3. 3 ng/L～10. 5 ng/L。平均回收率为80. 6%～91. 2%,RSD为4. 7%～8. 7%。结论聚吡咯修饰磁性纳米材料对喹诺酮类药物具有良好的吸附性能,结合HPLC-MS/MS,可用于富集、分离和测定环境水样中的11种喹诺酮类抗生素残留。
Objective To establish a solid-phase extraction method of separating and determining quinolones in water with polypyrrole（PPy）-coated Fe_3O_4 magnetic nanoparticles（Fe_3O_4@ PPy MNPs） and ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）. Methods The composite was synthesized through the chemical oxidation method,combining PPy role monomer with Fe_3O_4 magnetic ball in the form of aggregation state and the coated nanoparticlespossessed core-shell construction. The composite has been characterized by transmission electron microscopy（HPLC-MS/MS）.The pH value of water sample was adjusted to 4. 0 by formic acid. Then the microspheres were added,vortexed for 30 min and separated from the matrix by magnetic. The targets were eluted by 2 ml 10% Ammonia： MeOH（V/V）. Subsequently,the extract was dried under a gentle stream of nitrogen. The residue was re-dissolved with 0. 1% formic acid： MeOH（V/V）. The supernatant was filtered with 0. 22 μm membrane and detected by ultra-performance liquid chromatography-tandem mass spectrometry in MRM（＋） mode. Results The calibration curves of microcystins showed a good linearity in the range of5 ng/L-1 000 ng/L,with correlation coefficients above 0. 999 0. The LOD of the method were within 1. 1 ng/L-3. 5 ng/L and LOQ were within 3. 3 ng/L-10. 5 ng/L. The average recoveries ranged from 80. 6% to 91. 2%,with the relative standard deviation（RSD） of 4. 7%-8. 7%. Conclusion The results show that Fe_3O_4@ PPy MNPs has good adsorption properties for quinolones,and it can be used to enrich and separate 11 quinolones in water with HPLC-MS/MS.
作者
王芳
赵鸿雁
邵国健
朱文涛
WANG Fang;ZHAO Hong-yan;SHAO Guo-jian;ZHU Wen-tao(Huzhou Center for Disease Control and Prevention,Huzhou,Zhejiang 313000,China)
出处
《中国卫生检验杂志》
CAS
2018年第19期2316-2320,共5页
Chinese Journal of Health Laboratory Technology
关键词
聚吡咯
磁性固相萃取
喹诺酮
超高效液相色谱-串联质谱法
Potypyrrole
Magnetic solid - phase
Quinolone
Ultra performance liquid chromatography - tandem mass spectrometry
