Gao C X, Krull I S
Department of Chemistry, Northeastern University, Boston, MA 02115.
J Chromatogr. 1990 Aug 31;515:337-56. doi: 10.1016/s0021-9673(01)89329-8.
This paper introduces a novel polymeric dimethylaminopyridinium 9-fluorenyl-methoxycarbonyl reagent for off-line derivatizations of weak nucleophiles in high-performance liquid chromatography. The method of synthesis and characterization of the polymeric reagent via loading determinations is presented and discussed. Derivatization conditions (solvent, time, and temperature) for primary and secondary alcohols were optimized. As one application, off-line derivatizations of 2-chloro-1-propanol, a potential carcinogen in foodstuffs, were carried out with this polymeric reagent with single-blind and standard addition techniques. A specific sample treatment procedure was also developed. The accuracy and precision of the method were determined and data were statistically evaluated.
本文介绍了一种新型的聚合物二甲基氨基吡啶鎓9-芴甲氧羰基试剂，用于高效液相色谱中弱亲核试剂的离线衍生化。介绍并讨论了通过负载量测定来合成和表征该聚合物试剂的方法。对伯醇和仲醇的衍生化条件（溶剂、时间和温度）进行了优化。作为一种应用，使用该聚合物试剂通过单盲和标准加入技术对食品中的潜在致癌物2-氯-1-丙醇进行了离线衍生化。还开发了一种特定的样品处理程序。测定了该方法的准确度和精密度，并对数据进行了统计评估。
