热敏型可修复分子印迹固相微萃取纤维的制备及其应用
Preparation and application of thermosensitive and repairable molecularly imprinted solid phase microextraction fiber
-
摘要: 以螺旋霉素为模板分子，甲基丙烯酸和N-异丙基丙烯酰胺为功能单体，乙二醇甲基丙烯酸酯为交联剂，硅烷化的石英毛细管为载体合成了具有热敏型、可修复的分子印迹固相微萃取纤维。通过扫描电镜和氮气吸附/脱附对制备的分子印迹固相微萃取纤维进行表征，并对影响萃取效果的参数进行了优化。分子印迹固相微萃取纤维对大环内酯类抗生素具有高选择性和灵敏性，与高效液相色谱联用可对食品基质中的螺旋霉素、替米考星、泰乐菌素、交沙霉素4种大环内酯类抗生素进行定量分析，在0.5～50 μg/mL范围内，色谱峰面积与浓度呈良好的线性关系，样品在3种不同添加水平下的加标回收率在81.8%～119.1%之间，日间精密度均小于13.8%（n=6），日内精密度均小于15.5%（n=3）。Abstract: In this study,thermosensitive and repairable molecularly imprinted solid-phase microextraction fibers were synthesized using spiramycin as template molecule,methacrylic acid and N-isopropylacrylamide as functional monomers,ethylene glycol dimethacrylate as crosslinking agent,and silanized quartz capillary as carrier. The prepared molecularly imprinted solid-phase microextraction fibers were characterized by scanning electron microscope and nitrogen adsorption/desorption,and various parameters affecting the extraction efficiency were optimized. Due to high selectivity and sensitivity of the fibers for macrolide antibiotics,the quantitative analysis of four macrolide antibiotics in food matrix,spiramycin,tilmicosin,tylosin,and josamycin,was peroformed in combination with high performance liquid chromatography. In the range of 0.5 to 50 μg/mL,the chromatographic peak area showed a good linear relationship with the concentration. The spike recoveries of the samples at three different addition levels were between 81.8% and 119.1%;the inter-day precisions were less than 13.8% (n=6),and the intra-day precisions were less than 15.5% (n=3).
-
-
[1] . Int J Antimicrob Agents，2018，51（3）：283?298. [2] Zhang Y，Li XQ，Li HM，et al. Antibiotic residues in honey：a review on analytical methods by liquid chromatography tandem mass spectrometry［J］. Trac Trends Anal Chem，2019，110：344?356. [3] Du LJ，Yi L，Ye LH，et al. Miniaturized solid-phase extraction of macrolide antibiotics in honey and bovine milk using mesoporous MCM-41 silica as sorbent［J］. J Chromatogr A，2018，1537：10?20. [4] Senta I，Krizman-Matasic I，Terzic S，et al. Comprehensive determination of macrolide antibiotics，their synthesis intermediates and transformation products in wastewater effluents and ambient waters by liquid chromatography-tandem mass spectrometry［J］. J Chromatogr A，2017，1509：60?68. [5] Zhou YS，Zhou TT，Jin H，et al. Rapid and selective extraction of multiple macrolide antibiotics in foodstuff samples based on magnetic molecularly imprinted polymers［J］. Talanta，2015，137：1?10. [6] Zhou WE，Ling Y，Liu T，et al. Simultaneous determination of 16 macrolide antibiotics and 4 metabolites in milk by using Quick，Easy，Cheap，Effective，Rugged，and Safe extraction （QuEChERS） and high performance liquid chromatography tandem mass spectrometry［J］. J Chromatogr B Analyt Technol Biomed Life Sci，2017，1061/1062：411?420. [7] Song XQ，Zhou T，Liu QY，et al. Molecularly imprinted solid-phase extraction for the determination of ten macrolide drugs residues in animal muscles by liquid chromatography-tandem mass spectrometry［J］. Food Chem，2016，208：169?176. [8] Liu YH，Yang QX，Chen XT，et al. Sensitive analysis of trace macrolide antibiotics in complex food samples by ambient mass spectrometry with molecularly imprinted polymer-coated wooden tips［J］. Talanta，2019，204：238?247. [9] Diao XF，Zhang FF，Yang BC，et al. Preparation and evaluation of C10-cationic latex particle coated open-tubular column for capillary electrochromatography［J］. J Chromatogr A，2012，1267：127?130. [10] Xu LC，Pan JM，Dai JD，et al. Preparation of thermal-responsive magnetic molecularly imprinted polymers for selective removal of antibiotics from aqueous solution［J］. J Hazard Mater，2012，233/234：48?56. -
期刊类型引用(0)
其他类型引用(2)
计量
- 文章访问数: 160
- HTML全文浏览量: 10
- PDF下载量: 574
- 被引次数: 2
下载:
