基于混合吸附剂磁性固相萃取/高效液相色谱-串联质谱法测定水中磺胺和喹诺酮类抗生素残留  

Determination of Sulfonamides and Quinolones Antibiotics Residues in Water Samples by High Performance Liquid Chromatography-Tandem Mass Spectrometry with Mixed Adsorbents Based Magnetic Solid Phase Extraction

作　　者：魏丹 张菊 国明[2] WEI Dan;ZHANG Ju;GUO Ming(College of Bioscience and Engineering,Hebei University of Economics and Business,Shijiazhuang 050061,China;Center of Analysis and Testing,Zhejiang Research Institute of Chemical Industry Co.,Ltd.,Hangzhou 310023,China)

机构地区：[1]河北经贸大学生物科学与工程学院,河北石家庄050061 [2]浙江省化工研究院有限公司分析测试中心,浙江杭州310023

出　　处：《分析测试学报》2022年第2期187-195,共9页Journal of Instrumental Analysis

基　　金：河北省自然科学基金项目(H2020207002)。

摘　　要：通过制备磁性大孔有机共聚物材料(Fe_(3)O_(4)@Si O_(2)@PLS)和磁性金属有机骨架材料(Fe_(3)O_(4)@ZIF-8),将两种材料同时作为磁性吸附剂,建立了混合吸附剂磁性固相萃取/高效液相色谱-串联质谱(MSPE/HPLC-MS/MS)测定水中4种磺胺类和8种喹诺酮类抗生素残留的分析方法。通过扫描电子显微镜(SEM)、傅里叶变换红外光谱(FT-IR)和X-射线衍射仪(XRD)对两种磁性材料进行表面形貌和结构表征,结果显示,亲水亲脂大孔有机共聚物(PLS)包覆于磁性纳米粒子Fe_(3)O_(4)表面,且Fe_(3)O_(4)成功附着于正六边形金属有机骨架材料(ZIF-8)晶体表面,可以满足磁性固相萃取的要求。通过优化吸附剂用量、萃取方式、吸附时间、样品p H值、洗脱剂种类及洗脱时间,在最优的实验条件下,12种目标物的线性范围为0.5~10μg/L,相关系数(r^(2))为0.9961~0.9998,检出限(S/N=3)为0.01~0.14μg/L,定量下限(S/N=10)为0.04~0.45μg/L。所建方法成功用于水中12种目标抗生素的检测,在3个加标水平下的回收率为75.0%~107%,相对标准偏差(RSD)为0.50%~5.5%。该方法适用于水中痕量磺胺类和喹诺酮类抗生素残留的分析。A magnetic macroporous material(Fe_(3)O_(4)@Si O_(2)@PLS)and a metal organic framework composite(Fe_(3)O_(4)@ZIF-8)were synthesized in this paper,and they both were combined to use as a mixed magnetic adsorbent.Based on this,a high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)with the mixed magnetic adsorbent solid phase extraction(MSPE)was established for the quantitative analysis of 4 sulfonamides and 8 quinolones in water samples.The morphologies,chemical structure information and crystalline structures of the prepared materials were characterized by scanning electron microscopy(SEM),Fourier-transform infrared spectroscopy(FT-IR)and X-ray diffractometry(XRD).The results showed that the prepared Fe_(3)O_(4)@Si O_(2)@PLS appeared nearly spherical in shape,with a large specific surface and an average size of 500-600 nm,nearly without Fe_(3)O_(4)on the surface,suggesting the formation of core-shell structure Fe_(3)O_(4)@Si O_(2)@PLS,while Fe_(3)O_(4)@ZIF-8 was nearly spherical in shape,with an average diameter about 200 nm and a rough surface.The crystalline structures of Fe_(3)O_(4)and ZIF-8 in Fe_(3)O_(4)@ZIF-8 did not change after the preparation reaction,indicating that the spherical Fe_(3)O_(4)particles were unifomly attached to the surfaces of the orthohexagnal ZIF-8 crystals.And then the two magnetic nanoparticles were simultaneously introduced to extract 12 antibiotics residues in water samples by MSPE followed by HPLC-MS/MS.In order to establish the optimal extraction conditions,the key parameters influencing MSPE,i.e.magnetic adsorbent amount,adsorption mode,adsorption time,sample p H,elution solvent and elution time were investigated in detail.All the experiments were performed in parallel for three times.In the adsorption procedure of MSPE,12 antibiotics could be extracted completely by the mixture use of 35 mg Fe_(3)O_(4)@Si O_(2)@PLS and 15 mg Fe_(3)O_(4)@ZIF-8 within 10 min.Elution was performed using 10 m L 5%ammonia methanol for 5 min.The target compounds were separated on

关 键 词：混合磁性吸附剂 磁性固相萃取 高效液相色谱-串联质谱 抗生素残留 

分 类 号：O657.7[理学—分析化学] X132[理学—化学]