食品科学 ›› 2012, Vol. 33 ›› Issue (24): 205-209.doi: 10.7506/spkx1002-6630-201224042

• 分析检测 • 上一篇    下一篇

分子印迹固相萃取-化学发光法测定蔬菜中的马来酰肼

周敏,米娟,刘彩云 ,王树伦,马永钧   

  1. 西北师范大学化学化工学院,甘肃省生物电化学与环境分析重点实验室,甘肃省高分子材料重点实验室,省部共建生态环境相关高分子材料教育部重点实验室,甘肃 兰州 730070
  • 收稿日期:2011-09-20 修回日期:2012-11-07 出版日期:2012-12-25 发布日期:2012-12-12
  • 通讯作者: 周敏 E-mail:mzhou8367@sina.com
  • 基金资助:

    国家自然科学基金;甘肃省自然科学基金资助项目

Determination of Maleic Hydrazide in Vegetables by Molecularly Imprinting Solid Phase Extraction-Chemiluminescence Method

ZHOU Min,MI Juan,LIU Cai-yun,WANG Shu-lun,MA Yong-jun   

  1. Key Laboratory of Bioelectrochemistry and Environmental Analysis of Gansu Province, Key Laboratoryof Polymer Materials of GansuProvince, Key Laboratory of Eco-Environment-Related Polymer Materials, Ministry of Education, College of Chemistry and ChemicalEngineering, Northwest Normal University, Lanzhou 30070, China
  • Received:2011-09-20 Revised:2012-11-07 Online:2012-12-25 Published:2012-12-12
  • Supported by:

    the National Natural Science Foundation of China

摘要: 马来酰肼对高良姜素-高锰酸钾-多聚磷酸体系的化学发光具有增敏作用,据此结合分子印迹固相萃取技术建立测定蔬菜中马来酰肼含量的流动注射-化学发光分析方法。以马来酰肼为模板分子,甲基丙烯酸为功能单体,乙二醇二甲基丙烯酸酯为交联剂,偶氮二异丁腈为引发剂,用热聚合法合成了马来酰肼分子印迹聚合物,并以此分子印迹聚合物作为固相萃取填料制成固相萃取柱,对样品进行固相萃取后进行发光检测。在最优条件下,相对化学发光强度与马来酰肼的质量浓度在5.0×10-5~3.0×10-2mg/mL范围内呈良好的线性关系,检出限2.6×10-5mg/mL(3σ),相对标准偏差2.7%(1.0×10-3mg/mL马来酰肼,n=10)。将该法应用于马铃薯、洋葱及大蒜中马来酰肼含量的测定,加标回收率在95.2%~111.7%之间,相对标准偏差分别为1.8%、2.4%和2.1%。

关键词: 马来酰肼, 分子印迹, 固相萃取, 化学发光, 流动注射, 蔬菜

Abstract: A flow injection-chemiluminescence (FI-CL) method based on molecular imprinting-solid phase extraction has been developed for the determination of maleic hydrazide (MH) in vegetables. This method was based on the enhancement effect of MH on chemiluminescence intensity of galangin-potassium permanganate-polyphosphoric acid system. A molecular imprinting polymer (MIP) was synthesized from the thermally initiated polymerization of MH as a template molecule, methacrylic acid as a functional monomer and ethylene glycol dimethacrylate (EGDMA) as a cross-linker and azodiisobutyronitrile (AIBN) as an initiator and used to prepare a solid phase extraction column. Samples were subjected to solid phase extraction before CL assay. Under optimized conditions, relative CL intensity showed good linear relationship with MH concentration in the range from 5.0 × 10-5 to 3.0 × 10-2 mg/mL. The limit of detection of this method was 2.6 × 10-5 mg/mL (3σ). The precision (RSD) for 10 replicate determinations of a known concentration of MH (1.0 × 10-3 mg/mL) was 2.7%. In the determination of potato, onion and garlic by this method, average spike recovers of MH were in the range from 95.2% to 111.7% with RSD 1.8% for potato, 2.4% for onion and 2.1% for garlic, respectively.

Key words: maleic hydrazide (MH), molecular imprinting polymers (MIPs), solid phase extraction (SPE), flow injection (FI), chemiluminescence (CL), vegetables

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