核壳聚苯胺选择性磁性固相萃取-高效液相色谱-质谱法测定牛奶中痕量磺胺类药物  

Determination of Trace Sulfonamides Antibiotics in Milk Using Polyaniline Silicon Magnetic Composite Selective Magnetic Solid Phase Extraction Combined with High Performance Liquid Chromatography-Mass Spectrometry

作　　者：王泽岚 周艳芬 孟哲[1] 李吉光 李和平[1] 任建林[1] 刘万毅[1] WANG Ze-Lan;ZHOU Yan-Fen;MENG Zhe;LI Ji-Guang;LI He-Ping;REN Jian-Lin;LIU Wan-Yi(State Key Laboratory of High-Efficiency Utilization of Coal and Green Chemical Engineering, School of Chemistry and Chemical Engineering,Ningxia University,Yinchuan 750021,China)

机构地区：[1]宁夏大学化学化工学院省部共建煤炭高效利用与绿色化工国家重点实验室,银川750021

出　　处：《分析化学》2019年第1期119-128,共10页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金(No.21768003);西部地区建设一流大学的重大创新项目(No.ZKZD2017003);宁夏国内一流学科建设项目(No.NXYLXK2017A04)资助~~

摘　　要：采用低温(0℃)-原位氧化聚合-共沉淀法制备多层核壳聚苯胺硅磁复合物(Fe_3O_4@Si O_2@PANI)。将其作为磁性固相吸附剂用于选择性萃取和富集牛奶样品中4种痕量的磺胺类抗生素,结合高效液相色谱-质谱法进行测定。以透射电子显微镜、扫描电子显微镜、傅里叶变换红外光谱和振动样品磁力仪表征材料。通过响应曲面法,优化磁性固相萃取条件,得到最佳的萃取条件为:将15.0 mg Fe_3O_4@Si O_2@PANI分散于10 m L牛奶样品中,振荡40 min,磁性分离获取磁性吸附剂,用1 m L甲醇-水(7∶3,V/V)一步洗脱后待HPLC-MS分析。4种磺胺类化合物在10"1500μg/L范围内线性关系良好,相关系数为0.9976～0.9995,检出限为1.3"8.2#g/kg,3个加标浓度水平的回收率为69.7%"99.6%,日内RSDs为3.4%"4.6%,日间RSDs为7.8%"10.7%。本方法选择性好、灵敏度高、背景干扰低,适用于乳制品中痕量磺胺类抗生素的同时检测。The multi-layer core-shell polyaniline silicon magnetic composites(Fe 3O 4@SiO 2@PANI)were prepared in situ by oxidation polymerization-coprecipitation of silicon magnetic particles with low temperature(0℃).The Fe 3O 4@SiO 2@PANI was used as the adsorbent for the selective magnetic solid-phase extraction(MSPE)of four trace sulfonamides(SAs)antibiotics in milk samples prior to high performance liquid chromatography with mass spectrometry(HPLC-MS).The synthesized nanocomposite sorbents were characterized by Fourier transform infrared spectra(FT-IR),scanning electron microscopy(SEM),transmission electron microscopy(TEM),and vibrating sample magnetometry(VSM)techniques.The predominant variables affecting the extraction efficiency of the MSPE procedure were investigated and optimized via the response surface methodology.The optimal conditions for separation and preconcentration of trace sulfonamides in milk sample were as follows.About 15.0 mg of Fe 3O 4@SiO 2@PANI was dispersed into 10 mL of milk sample and shaken for 40 min.Then,the Fe 3O 4@SiO 2@PANI carrying sulfonamides was separated from the milk sample by an external magnetic field.Next,the sulfonamides were eluted from Fe 3O 4@SiO 2@PANI with 1.0 mL of methanol aqueous solution(7∶3,V/V).Under the optimized conditions,an excellent linearity was observed in the range of 10-1500μg/L for the four sulfonamides,with the correlation coefficients of 0.9976-0.9995.The limits of detections ranged from 1.3 ~8.2 ug/kg.The mean recoveries at three spiked levels ranged from 69.7%to 99.6%.The relative standard deviations(RSDs)of intra-day and inter-day varied from 3.4%to 4.6%and 7.8%to 10.7%,respectively.The proposed method had low background and high selectivity and sensitivity,and was successfully applied to the simultaneous determination of four kinds of trace sulfonamides antibiotics in milk sample.

关 键 词：硅磁聚苯胺 磁性固相萃取 磺胺类抗生素 高效液相色谱-串联质谱 

分 类 号：O657.63[理学—分析化学] TS252.7[理学—化学]