食品中痕量低分子量挥发性有机物高效富集及表面增强拉曼光谱现场分析新技术研究

It is difficult to enrich low molecular weight volatile organic compounds (VOCs) due to their extremely strong volatility at room temperature. Study of novel efficient enrichment techniques for trace low molecular weight VOCs in complicated samples is one of bottle necks in the field of sample preparation. The key to achieve rapid, accurate, quantitative on-site analysis of low molecular weight VOCs lays on the development of novel enrichment methods with high selectivity coupled with corresponding portable rapid analytical technique. In this project novel enrichment media with high selectivity and related enrichment-sampling techniques for low molecular weight VOCs in food will be developed based on some novel gas absorption materials such as inorganic crystals - polymer doped, bimetallic catalyst, nano composite metal oxide material. The target VOCs focus on trace formaldehyde, ethylene and ethanol which take great concern in field of food security analysis. Combined with homemade sampling devices and portable surface enhanced raman scattering (SERS) instrument, new on-site analytical techniques for the rapid, accurate and quantitative analysis of formaldehyde, ethylene and ethanol in food samples will be established. The new on-site analytical techniques will be actually used for the real-time and accurate quantitative analysis of low molecular weight VOCs during food storage, transportation and fermentation process. It is expected to develop the novel on-site and quantitative analytical technique for low molecular weight VOCs in food which can be actually applied in food security analysis through the studies in this project.

挥发性有机物（VOCs）常温下极易挥发逃逸、不易富集，复杂样品中痕量低分子量VOCs高效富集新技术研究是样品预处理领域的难点之一。研发高选择性低分子量VOCs富集新方法，并结合相应便携快速分析技术，是实现低分子量VOCs快速、准确、定量现场分析的关键。本项目拟针对食品中痕量甲醛、乙烯、乙醇等低分子量VOCs，基于无机晶体-高聚物掺杂、双金属催化、纳米复合金属氧化物等新型气体吸附材料设计合成高选择性低分子量VOCs富集介质，构建痕量低分子量VOCs高选择性富集采样新方法 ；结合自制采样装置及便携的表面增强拉曼（SERS）仪器，建立食品中甲醛、乙烯及乙醇等痕量低分子量VOCs快速、准确、定量现场分析新技术，并实际用于食品运输储藏、发酵酿造等过程中痕量低分子量VOCs的实时准确定量分析。通过本项目有望研发食品中低分子量VOCs现场定量分析新技术，并实际用于食品安全分析。

表面增强拉曼光谱（SERS）技术灵敏度高、检测速度快、仪器便携、试剂消耗量少、能反映待测分子结构、具备多组分同时检测潜力，因此在食品安全快速分析中有着广阔的应用前景。食品中低分子量挥发性有机物（VOCs）是质量控制及食品安全分析中的重要标志物，但由于此类化合物挥发性强、含量低，且食品样品基体干扰严重，SERS检测信号重现性欠佳，目前缺乏相应的快速定量分析方法。通过研发高容量、高选择性低分子量VOCs富集介质，结合便携采样装置，可以实现食品中低分子量VOCs的高效富集，且能有效去除基体干扰，结合SERS等快检技术，有望提高食品低分子量VOCs快速分析的重现性及准确性，实现食品中低分子量VOCs的快速、准确、定量现场分析。. 项目按原计划圆满顺利完成，并达到预期目标。采用层层键和法、电化学原位聚合法、化学原位嵌入法等制备技术，研制得金属有机框架化合物MOF-199/碳纳米管（MOF-199/CNTs）、磺化石墨烯/聚吡咯（SG/PPy）、三氧化钼/聚吡咯（MoO3/PPy）等多种高容量、高选择性低分子量VOCs富集介质；采用原子转移自由基聚合法结合交联技术制备金-聚苯乙烯（Au@PS-OH）纳米阵列SERS基底。研制了大体积恒浓度（LVCC）气体采样装置及微型热助吹扫捕集（MTPTD）装置等便携低分子量VOCs采样技术。结合SERS等检测技术，成功构建了水产品及面粉中甲醛、水果中植物激素乙烯、水果保鲜气中二氧化硫、酒精制品中甲醇、味精中硫化钠、植食性香料作物萜类VOCs等食品安全分析关注的典型痕量低分子量VOCs的快速定量分析方法。在Analytical Chemistry等国内外刊物上发表学术论文及综述14篇，申请发明专利4项，培养博士生2名、硕士生6名。

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