色谱

色谱 ›› 2012, Vol. 30 ›› Issue (01): 56-61.DOI: 10.3724/SP.J.1123.2011.08033

• 研究论文 • 上一篇    下一篇

分子印迹固相萃取-高效液相色谱法测定饲料中莱克多巴胺

黄怡, 张青杰, 刘敏, 王旭峰, 李建琴, 贺利民*   

  1. 华南农业大学兽医学院兽医药理研究室, 广东 广州 510642
  • 收稿日期:2011-08-22 修回日期:2011-10-06 出版日期:2012-01-28 发布日期:2012-03-01
  • 通讯作者: 贺利民,博士,副研究员,主要从事食品质量安全分析检测技术研究. Tel: (020)85284896,
  • 基金资助:

    国家自然科学基金项目(31072166).

Molecularly-imprinted solid phase extraction coupled with high performance liquid chromatography for the determination of ractopamine in feed samples

HUANG Yi, ZHANG Qingjie, LIU Min, WANG Xufeng, LI Jianqin, HE Limin*   

  1. Department of Veterinary Pharmacology and Toxicology, College of Veterinary Medicine, South China Agricultural University, Guangzhou 510642, China
  • Received:2011-08-22 Revised:2011-10-06 Online:2012-01-28 Published:2012-03-01

PDF

476

被引次数

92

摘要： 以莱克多巴胺为模板分子,丙烯酰胺为功能单体,乙二醇二甲基丙烯酸酯为交联剂,合成了对莱克多巴胺具有高选择性的分子印迹聚合物。考察了甲醇、乙腈、丙酮和氯仿-甲醇与三乙胺构成致孔剂合成的聚合物性能及其形貌特征。通过正交试验优化的聚合反应配方为: 1.0 mmol莱克多巴胺,4.0 mmol丙烯酰胺,20.0 mmol乙二醇二甲基丙烯酸酯,6.0 mL乙腈-三乙胺(30:1, v/v), 50.0 mg偶氮二异丁腈。建立的基于分子印迹固相萃取-高效液相色谱测定饲料试样中莱克多巴胺的方法,在0.50～100 mg/L质量浓度范围内有良好的线性关系(r=0.9994);饲料试样中1.0、10及100 mg/kg 3个添加水平的莱克多巴胺平均回收率大于80%;批内、批间测定的相对标准偏差小于10%;检出限(信噪比为3)达到0.1 mg/kg。该方法灵敏、可靠,用于饲料等复杂基质中莱克多巴胺检测的效果优于相关标准分析方法。

关键词: 分子印迹聚合物, 高效液相色谱, 固相萃取, 莱克多巴胺, 饲料

Abstract: Molecularly imprinted polymers (MIPs) with high selectivity to ractopamine (RAC) were prepared by using RAC as template, acrylamide (AM) as monomer, and ethylene glycol dimethacrylate (EGDMA) as cross-linker. The effects of four porogens (methanol, acetonitrile, acetone, and chloroform-methanol) with triethylamine (30:1, v/v) on the recognition capability of MIPs to RAC and the morphological characteristics of the polymers were investigated. Orthogonal test was used to optimize the preparation of MIPs, and the optimal compositions were as follows: 1.0 mmol RAC, 4.0 mmol AM, 20.0 mmol EGDMA, 6.0 mL acetonitrile-triethylamine (30:1, v/v), and 50.0 mg azobisisobutyronitrile. A high performance liquid chromatographic method based on molecularly-imprinted solid-phase extraction (MISPE) was developed for the determination of ractopamine in feed samples. The limit of detection (LOD, S/N=3) of ractopamine was 0.1 mg/kg. The linear range was 0.50~100 mg/L (r=0.9994). Mean recoveries of RAC spiked in 3 kinds of feed samples at 1.0, 10 and 100 mg/kg were above 80% with the relative standard deviations of less than 10%. The clean-up efficiency of MISPE was ideal for feed samples. The method is more sensitive and reproduciable than the standard analytical method for the determination of RAC in feed matrices.

Key words: feeds, high performance liquid chromatography (HPLC), ractopamine, solid-phase extraction (SPE), molecularly imprinted polymers (MIPs)