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A Novel Solid Phase Derivatization Reagent for the Determination of Amines by Gas Chromatography-Flame Ionization Detection.

机译：气相色谱-火焰电离检测用于测定胺的新型固相衍生试剂。

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摘要

Combinatorial chemistry is a powerful tool in developing chemical libraries, which undergo high-throughput screening for potential drug leads, catalysts and materials. To address this demand, large combinatorial libraries of peptides, oligonucleotides, and other organic compounds have been developed based on solid phase synthesis (SPS). Polystyrene is the most popular SPS support for the majority of peptide synthesis while silica is preferred for oligonucleotides synthesis, but less frequently investigated. We have explored silica as a SPS support since it is inexpensive and has a higher coupling rate than polystyrene. Slica-bound 1-hydroxybenzotriazole (Si-HOBt) and polystyrene-bound 1-hydroxybenzotriazole (P-HOBt) based solid supports were prepared. Using these supports, a small combinatorial library of acetamides and benzamides were synthesized. Acetamides were obtained in higher yield irrespective of the solid support. Silica based synthesis had better yield of benzamides in comparison to polystyrene based synthesis. Besides this, Si-HOBt had retained a higher activity after five reuses. Therefore, Si-HOBt was chosen for further applications in analytical chemistry.;Biogenic amines are precursors of carcinogenic N-nitroso compounds, and have been reported to cause liver cirrhosis, muscular dystrophy, diabetes, Alzheimer's disease and scombroid food poisoning. Hence, it is imperative that biogenic amines be monitored in food samples. Analysis of biogenic amines by gas chromatography-flame ionization detection (GC-FID) exhibits peak tailing and adsorption on to the columns. To overcome these problems, Si-HOBt based solid phase analytical derivatization (SPAD) was performed to convert the biogenic amines into a thermally stable, non-polar benzamides. Each analyte was individually tested for SPAD. Later, the mixture of biogenic amines were collectively derivatized and analyzed by GC-FID. SPAD was optimized with respect to solvent, time, quantity of the reagent and mode of derivatization. In addition, the SPAD was validated by the determination of biogenic amines in tuna and mackerel. A two week study of mackerel sample at 3, 21 and 37 °C showed increasing peak areas and varying concentrations of tyramine and phenethylamine. The details of development, optimization and validation of SPAD will be discussed.
机译：组合化学是开发化学库的强大工具，化学库经过高通量筛选，可筛选潜在的药物前导物，催化剂和材料。为了满足该需求，已经基于固相合成（SPS）开发了肽，寡核苷酸和其他有机化合物的大型组合库。聚苯乙烯是大多数肽合成中最受欢迎的SPS支持物，而二氧化硅则是寡核苷酸合成的首选，但研究频率较低。我们已经研究了二氧化硅作为SPS载体，因为它便宜且偶联率比聚苯乙烯高。制备了基于滑石的1-羟基苯并三唑（Si-HOBt）和基于聚苯乙烯的1-羟基苯并三唑（P-HOBt）。使用这些支持物，合成了乙酰胺和苯甲酰胺的小型组合库。不管固体载体如何，都以较高的产率获得乙酰胺。与基于聚苯乙烯的合成相比，基于二氧化硅的合成具有更好的苯甲酰胺收率。除此之外，Si-HOBt在重复使用五次后仍保留了较高的活性。因此，选择了Si-HOBt进一步用于分析化学中。生物胺是致癌的N-亚硝基化合物的前体，并且据报道会引起肝硬化，肌肉营养不良，糖尿病，阿尔茨海默氏病和类固醇食物中毒。因此，必须对食品样品中的生物胺进行监测。通过气相色谱-火焰电离检测（GC-FID）分析生物胺时，峰拖尾和吸附在色谱柱上。为了克服这些问题，进行了基于Si-HOBt的固相分析衍生化（SPAD），将生物胺转化为热稳定的非极性苯甲酰胺。对每种分析物分别进行SPAD测试。之后，将生物胺的混合物共同衍生化并通过GC-FID进行分析。在溶剂，时间，试剂数量和衍生方式方面对SPAD进行了优化。此外，通过测定金枪鱼和鲭鱼中的生物胺来验证SPAD。对鲭鱼样品在3、21和37°C下进行的为期两周的研究表明，峰面积增加，酪胺和苯乙胺的浓度变化。将讨论SPAD的开发，优化和验证的细节。

著录项

  • 作者

    Vokkaliga, Smitha A.;

  • 作者单位

    University of Maryland, Baltimore County.;

  • 授予单位 University of Maryland, Baltimore County.;
  • 学科 Chemistry Analytical.;Chemistry Polymer.;Chemistry Organic.
  • 学位 Ph.D.
  • 年度 2011
  • 页码 154 p.
  • 总页数 154
  • 原文格式 PDF
  • 正文语种 eng
  • 中图分类
  • 关键词

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