色谱

色谱 ›› 2014, Vol. 32 ›› Issue (11): 1214-1218.DOI: 10.3724/SP.J.1123.2014.07001

• 研究论文 • 上一篇    下一篇

微囊藻毒素分子印迹搅拌棒涂层的研制及其吸附性能

丘秀珍1, 梁勇2, 郭会时1   

  1. 1. 韶关学院化学与环境工程学院, 广东 韶关 512005;
    2. 华南师范大学化学与环境学院, 广东 广州 510006
  • 收稿日期:2014-07-01 修回日期:2014-08-13 出版日期:2014-11-08 发布日期:2014-10-31
  • 通讯作者: 郭会时,E-mail:guohuishi@163.com.
  • 基金资助:

    国家自然科学基金项目(21071099);教育部留学回国人员科研启动基金(第39批);韶关市科技计划项目(2012140544).

Preparation of microcystin-LR molecularly imprinted polymer coated stir bar and its adsorptive performances

QIU Xiuzhen1, LIANG Yong2, GUO Huishi1   

  1. 1. College of Chemistry and Environmental Engineering, Shaoguan University, Shaoguan 512005, China;
    2. College of Chemistry and Environment, South China Normal University, Guangzhou 510006, China
  • Received:2014-07-01 Revised:2014-08-13 Online:2014-11-08 Published:2014-10-31

PDF

246

被引次数

3

摘要：

以微囊藻毒素(MC)-LR为模板,甲基丙烯酸(MAA)为功能单体,通过可逆加成-断裂链转移(RAFT)自由基聚合技术,在凹凸棒土(ATP)表面制备了磁性分子印迹聚合物,并通过溶胶-凝胶法将分子印迹聚合物作为涂层介质制作搅拌棒。同时通过红外吸收光谱和扫描电镜等对印迹聚合物进行了结构和形貌的表征,并用液相色谱研究了搅拌棒涂层对水体中微囊藻毒素的吸附性能。结果表明,在最佳萃取条件下,分子印迹搅拌棒涂层对MC-LR具有较高的选择性能,在0.010~5.0 mg/L范围内线性关系良好(r2>0.997),检出限(S/N=3)可低至0.27 μg/L。MC-LR加标水平为20.0~80.0 μg/L的回收率范围为83.33%~100.07%,相对标准偏差(RSD)为1.40%~9.17%。该方法快速、灵敏、选择性高,可用于环境水体中微囊藻毒素的分析检测。

关键词: 凹凸棒土, 磁性分子印迹聚合物, 搅拌棒吸附萃取, 可逆加成-断裂链转移自由基聚合, 微囊藻毒素-LR

Abstract:

An effective method for the preparation of magnetic molecularly imprinted polymers (MIPs) on attapulgite (ATP) using microcystin-LR (MC-LR) as template molecule through reversible addition fragmentation chain transfer (RAFT) radical polymerization was reported. A novel MIPs stir bar sorptive extraction (SBSE) coating was prepared by sol-gel method. The structure and morphology of MIPs were characterized by infrared spectroscopy (IR) and transmission electron microscopy (TEM). The adsorption performance of SBSE coated with MC-LR was studied by high performance liquid chromatography (HPLC). The results showed that under the optimized experimental conditions, the present method has high selectivity to MC-LR. A good linearity was achieved for MC-LR over the range of 0.010-5.0 mg/L and the limit of detection (S/N=3) was found to be as low as 0.27 μg/L. The proposed method was successfully applied to the determination of MC-LR in water samples. The average recoveries ranged from 83.33% to 100.07% with the relative standard deviations (RSDs) of 1.40%-9.17% at three spiked levels (20, 40 and 80 μg/L). The developed method is rapid, selective and sensitive, and adapts to the analysis of trace MC in water samples.

Key words: attapulgite (ATP), magnetic molecularly imprinted polymer, microcystin-LR (MC-LR), reversible addition fragmentation chain transfer (RAFT), stir bar sorptive extraction (SBSE)

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