基于溶胶-凝胶技术的乐果分子印迹固相微萃取涂层的评价及应用
目的 对溶胶-凝胶法制备的乐果分子印迹固相微萃取头进行评价, 并建立分子印迹固相微萃取与气相色谱联用(molecularly imprinted polymer-solid phase microextraction/gas chromatography, MIP-SPME/GC)检测环境水中乐果残留量的方法。方法 以非印迹(nonimprinted polymer, NIP)SPME萃取头为参照, 考查乐果分子印迹(MIP)萃取头的使用性能; 优化SPME萃取条件后, 对MIP-SPME/GC方法的分析性能进行评价, 最后检测实际样品。结果 该MIP萃取头的热稳定性和化学稳定性高, 在水相中萃取选择性好。在优化条件下, 方法在蒸馏水中线性范围为12.5~2500 μg/L, 线性相关系数为0.9997, 检出限为97.0 ng/L, 5次重复实验所得RSD为6.45%。应用本方法测定湖水和自来水中乐果含量, 均未有乐果检出。自来水中方法的加标回收率在92.0%~114.2%之间, 湖水中加标回收率为88.9%~102.1%。结论 溶胶-凝胶分子印迹SPME萃取头具有很高的操作稳定性, 能够用于水相识别。本方法简便、精密度高、准确度好, 在富水样品的乐果检测中具有明显优势。
Objective To evaluate a sol-gel coated molecularly imprinted polymer (MIP) fiber for solid-phase microextraction (SPME) and to establish a method for determination of dimethoate in environmental water by molecularly imprinted polymer-solid phase microextraction coupled with gas chromatography. Methods The characteristics of the MIP fiber was evaluated in comparison with the nonimprinted polymer (NIP) fiber. After optimization of extraction parameters, the method was evaluated through determination of dime-thoate in tap water and lake water. Results At the optimum conditions, the new fiber exhibited desirable thermal stability and chemical durability, and had a good selective extraction ability for dimethoate in water sample. The proposed method was linear in the range of 12.5~2500 μg/L with a coefficient of 0.9997. The limit of detection was 97.0 ng/L. The relative standard deviation of 5 replicates was 6.45%. Satisfactory recoveries of 92.0%~114.2% were obtained in tap water and 88.9%~102.1% in lake water. Conclusion The MIP-SPME fiber obtained has a good stability and performs well in aqueous recognition. This method is simple, reliable, and accurate, and is suitable for determination of dimethoate in water samples.
标题：基于溶胶-凝胶技术的乐果分子印迹固相微萃取涂层的评价及应用
英文标题：Evaluation and application of molecularly imprinted solid-phase microextraction fiber for detection of dimethoate based on sol-gel technique
作者：
李曌 环境食品学教育部重点实验室华中农业大学食品科学技术学院;武汉市蔡甸区农产品质量安全检验检测站
张雪娜 青岛京诚检测科技有限公司
李秀娟 环境食品学教育部重点实验室华中农业大学食品科学技术学院
中文关键词:溶胶-凝胶,分子印迹,固相微萃取,乐果,
英文关键词:sol-gel,molecularly imprinted polymer,solid phase microextraction,dimethoate,
发表日期：2015-11-06
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