多次顶空固相微萃取-气相色谱法检测泡菜中的氨基甲酸乙酯.docVIP

 多次顶空固相微萃取-气相色谱法检测泡菜 中的氨基甲酸乙酯# 张雪娜，雷芬芬，高远莉，汪雨龙，李秀娟** 5 10 15 20 25 30 35 40 （华中农业大学食品科学技术学院，武汉 430070） 摘要：建立了多次顶空固相微萃取/气相色谱（Multiple HS-SPME/GC）定量检测泡菜中的氨 基甲酸乙酯（EC）的方法。与几种商用涂层相比，自制的溶胶-凝胶苯胺甲基三乙氧基硅烷 -甲基丙烯酸/羟基硅油涂层对 EC 有很高的萃取效率。即便如此，由于 EC 很强的亲水性使 其萃取量太低，导致 Multiple HS-SPME 无法应用。在样品中添加足量的无水硫酸钠解决了 这一难题。常规 SPME 分析表明不同泡菜基质之间差异显著，而 Multiple HS-SPME 通过完 全萃取目标物有效消除了基质差异的影响，采用外标标准曲线法即可定量。在优化条件下， 方法的线性范围为 0.1-100 mg L-1，线性相关系数为 0.9996，检测限为 0.038 mg L-1，相对 标准偏差为 4.25%。在 5 种泡菜中加标，回收率在 91.2-104.2%之间，且检测结果与标准加 入法所得结果一致。实验表明，Multiple HS-SPME 方法简单、快速、准确、成本低，可以 有效克服基质差异的影响，尤其适合于大量复杂基质固体样品的定量分析。 关键词：分析化学；多次顶空固相微萃取；氨基甲酸乙酯；泡菜；基质干扰；气相色谱 中图分类号：O658 Determination of ethyl carbamate in pickles using multiple headspace solid-phase microextraction coupled with gas chromatography ZHANG Xuena, LEI Fenfen, GAO Yuanli, WANG Yulong, LI Xiujuan (College of Food Science Technology, Huazhong Agricultural University, Wuhan 430070) Abstract: A method has been developed for the quantitative determination of ethyl carbamate (EC) in pickles based on multiple headspace solid-phase microextraction (Multiple HS-SPME) coupled with gas chromatography. A novel anilino-methyl triethoxy silicane-methacrylic acid/terminated silicone oil (AMTEOS-MA/OH-TSO) fiber was developed by sol-gel technology and proved to be more efficient to EC than several commercial ones. An important problem still remained. The adsorption of EC by water in the samples caused low transport of analyte to the headspace, which made multiple HS-SPME invalidated. Mixing with anhydrous sodium sulphate, the sensitivity of the method was improved and the problem was solved. Serious matrix interference was observed among various types of pickles when the common SPME procedure was performed and multiple HS-SPME avoided the matrix effect by a complete recovery of the analytes. The linear range of the proposed method was 0.1-100 mg L-1, with a correlation coefficient of 0.9996. The precision gave satisfactory outcome of 4.25 % (n=5). The limit of