色谱

色谱

• 特别策划 • 上一篇    下一篇

聚(甲基丙烯酸-乙二醇二甲基丙烯酸酯)搅拌棒吸附萃取与液相色谱-质谱联用检测牛奶中的磺胺类药物

马乔1,2, 余琼卫1, 罗彦波1, 冯钰锜1*   

  1. (1. 生物医学分析化学教育部重点实验室(武汉大学), 武汉大学化学系, 湖北 武汉 430072; 2. 聚光科技(杭州)股份有限公司, 浙江 杭州 310052
  • 收稿日期:2011-01-09 修回日期:2011-02-15 出版日期:2011-07-28 发布日期:2011-08-19
  • 通讯作者: 冯钰锜,教授,博士生导师. Tel: (027)68755595
  • 基金资助:

    国家自然科学基金项目(91017013, 21005057, 31070327)

Stir rod sorptive extraction with poly(methacrylic acid-co-ethylene dimethacrylate) as coating and its application to the analysis of sulfonamides in milk samples

MA Qiao1,2, YU Qiongwei1, LUO Yanbo1, FENG Yuqi1*   

  1. 1. Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072, China; 2. Focused Photonics (Hangzhou), Inc., Hangzhou 310052, China
  • Received:2011-01-09 Revised:2011-02-15 Online:2011-07-28 Published:2011-08-19

PDF

508

被引次数

15

摘要： 将聚(甲基丙烯酸-乙二醇二甲基丙烯酸酯) (poly(MAA-co-EDMA))聚合物原位聚合于玻璃内插管外表面上,得到一种多孔聚合物涂层;将其作为搅拌棒吸附萃取的萃取介质,考察了其对磺胺类药物的萃取性能;最后将其与高效液相色谱-电喷雾质谱(HPLC-ESI-MS)联用,建立了一种牛奶中4种磺胺类药物的检测方法。在最佳条件下,牛奶中4种磺胺类药物的检出限(S/N=3)和定量限(S/N=10)分别为0.11～0.52 μg/L和0.35～1.72 μg/L。在1～500 μg/L的范围内峰面积与质量浓度具有良好的线性关系,日内、日间测定的相对标准偏差不高于11.3%。结果表明,该方法简便、灵敏度高且成本低,适合于牛奶中磺胺类药物的检测。

关键词: 磺胺类药物, 搅拌棒吸附萃取, 聚(甲基丙烯酸-乙二醇二甲基丙烯酸酯)聚合物, 牛奶

Abstract: A poly(methacrylic acid-co-ethylene dimethacrylate) polymer (poly(MAA-co-EDMA)) was prepared via in-situ polymerization on the outside surface of vial glass insert and used as stir rod sorptive extraction (SRSE) coating. The extraction performance of the polymer coating toward four sulfonamides (SAs) was investigated. The effects of several parameters to SRSE, such as the pH value, inorganic salt and organic phase concentrations of the sample matrix, were investigated. It demonstrated that the sulfonamides were captured on the poly(MAA-co-EDMA) coating mainly through cation-exchange and hydrophobic interactions. A novel approach is presented for the determination of four sulfonamide antibacterial residues in milk samples by coupling SRSE to liquid chromatography and electrospray ionization mass spectrometry (SRSE/LC-ESI-MS). In this method, the detection limits (S/N=3) of 0.11~0.52 μg/L and quantification limits (S/N=10) of 0.35~1.72 μg/L were obtained. The method showed good linearity in the range of 1~500 μg/L. Good method reproducibility was also found by intra- and inter-day precisions, yielding the relative standard deviations (RSDs) less than 11.3%. The results demonstrated that the proposed method is simple, sensitive, low cost and suitable for the determination of sulfonamides in milk samples.

Key words: milk, poly(methacrylic acid-co-ethylene dimethacrylate) (poly(MAA-co-EDMA)), sulfonamides (SAs), stir rod sorptive extraction (SRSE)