在线场辅助样品前处理-液相色谱联用技术及其应用研究

With the development of analytical instruments and analysis technology, rapid and efficient sample preparation plays an essential role in analytical methodology. Most analytical instruments are difficult to handle matrix directly and some forms of pretreatment are required to extract and to isolate the analytes. The solid sample pretreatment devices development lags behind, has become the significant problem in the process of analysis. Simultaneous performed microwave, ultrosonic and heat field would utilize the vastly accelerated extraction rate provided by field synergy effect. In the present project, a novel one-step sample preparation technique based on the field synergy integrated extraction and clean-up device is developed, in which the whole procedure is accelerated by field synergy, and no further cleanup or filtration precedes chromatographic analysis. The field synergy extraction tube is designed and an online coupled techenique based on field synergy extraction and liquid chromatography is developed; The online coupled method is applied on the analysis of heterocyclic amines in fried foods, organophosphorus in Traditional Chinese Medicines and sulfonamides in environmental samples.

样品前处理是复杂基体中痕量目标物分析检测的关键环节，发展快速高效的在线样品前处理-分析检测联用技术可提高分析方法的灵敏度、准确度和重现性。与气体和液体样品相比，固体样品的在线前处理/分离分析联用技术和联用装置的发展滞后。本项目针对固体样品因无法快速高效萃取、分离、富集而与后续分析方法难以实现在线分析的突出问题，拟采用微波场、热场和超声场等外场驱动力，通过场协同效应强化分析样品前处理中的传热和传质过程，研制适合固体样品在线分析检测的场辅助样品前处理装置；结合固相分散萃取、固相萃取等建立在线场辅助样品前处理-液相色谱联用技术；开展该联用技术在煎炸食品2-氨基-3-甲基咪唑[4,5-f]喹啉等杂环胺类、环境样品中磺胺喹噁啉等磺胺类抗生素和中药中有机磷类农残分析等领域中的应用研究。

样品前处理是复杂基体中痕量目标物分析检测的关键环节，发展快速高效的在线样品前处理-分析检测联用技术可提高分析方法的灵敏度、准确度和重现性。本项目围绕基于微波、超声波等场（协同）作用的样品前处理-微分离-液相色谱在线联用装置研制、联用技术开发及其应用开展研究。① 设计研制了玻璃、PEEK材料的3种场辅助萃取管；研制了场辅助、微分离和色谱在线联用接口，分别构建了微分离-色谱在线联用和场辅助-微分离-液相色谱在线联用装置。② 发展了场辅助萃取-SPE-HPLC在线分析技术和μSPE-HPLC在线分析技术，研究了该技术在食品中杂环胺，环境中多环芳烃，日用化妆品中糖皮质激素/抗生素等样品分析中的应用；烤肉中2-氨基-3-甲基咪唑[4,5-f]喹啉等5种杂环胺等检出限低至0.10-0.15 ng/L；烤土豆、烤鱼等样品中苯并[a]蒽、苯并[a] 芘等9种PAHs的检出限低至1.5 ng/kg。③ 结合实验与理论模拟研究了场辅助样品前处理的作用机理。通过正交实验和Comsol软件模拟研究了场效应、温度等因素对样品中痕量分析物萃取效率的影响；对比了不同场作用及其协同作用下痕量分析物的萃取性能。实验和理论模拟结果均表明场（协同）效应能有效提高分析物萃取效率。④ 拓展了磁场、电场等场作用在植物激素、环境污染物等痕量组分分析中的应用。研究结果证明，基于微波场、超声场、磁场、电场等场辅助-微分离-色谱在线联用技术可以有效减少分析误差、提高分析灵敏度，在食品安全、环境监测、药物研发、精细化工等领域有广泛的应用前景。.通过项目资助，先后研制场辅助萃取管2套；场辅助萃取-SPE-HPLC在线联用装置2套；发表文章10篇；申请发明专利2件；参加国内外学术会议11场次；培养高层次分析人才6人。