A simple, convenient, and efficient preparative GC system that uses a short megabore capillary column as a trap
A simple, convenient, and efficient preparative GC system that uses a short megabore capillary column as a trap
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DOI：
10.1007/s10886-008-9437-z
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发表时间：
2008-03-01
影响因子：
2.3
通讯作者：
Schal, Coby
中科院分区：
文献类型：
--
作者：
Nojima, Satoshi;Apperson, Charles S.;Schal, Coby
开发了一种简单、方便、高效的制备型GC系统，该系统使用短小的大孔毛细管柱作为样品采集(吸附剂)捕集器。以C4-C20正构烷烃、酯和醇为模型化合物，系统考察了不同类型毛细管柱捕集器在不同收集条件下的性能。吸附固定相的厚度和极性以及捕集器的温度影响捕集器的性能。每组化合物都被有效地捕获在一个临界的Kovat指数以上，并且陷阱的类型(失活的、甲基聚硅氧烷、聚乙二醇)、膜厚度以及陷阱是否被冷却都显著地改变了这个阈值指数。在这一临界指标以上，甲基聚硅氧烷薄膜捕集器在较大的注入样品质量范围内的回收率为80%-100%。例如，一个膜厚为1.5微米的DB-1聚硅氧烷捕集器在常温下工作，捕获所有三个化学类别的进样化合物质量的84%，科瓦特指数为1,100(在非极性色谱柱上测定)，进样质量从每种化合物的10到1,000纳克不等。对于大多数研究人员来说，这种制备型GC系统在技术和经济上都是可行的。此外，它还适用于制备挥发性和半挥发性化合物的核磁共振样品，特别是样品大小从几纳克到几微克的样品。
A simple, convenient, and highly efficient preparative GC system has been developed that uses short sections of megabore capillary columns as sample collection (sorbent) traps. The performance of this system with various types of capillary column traps and under various collection conditions was systematically investigated with model compounds, including C4 to C20 normal alkanes, esters, and alcohols. The thickness and polarity of the sorptive stationary phase and the temperature of the collection trap affected trap performance. Each group of compounds was efficiently trapped above a critical Kovat's index, and the type of trap (deactivated, methyl polysiloxane, polyethylene glycol), film thickness, and whether or not the trap was cooled significantly shifted this threshold index. Above this critical index, recovery efficiencies of traps with methyl polysiloxane films were 80-100% for a wide range of injected sample mass. For example, a DB-1 collection trap with a film thickness of 1.5 mu m methyl polysiloxane operated at ambient temperature trapped > 84% of the mass of injected compounds of all three chemical classes with Kovat's index > 1,100 (determined on a nonpolar column) with injected sample mass ranging from 10 to 1,000 ng of each compound. This preparative GC system is technically and economically feasible for most researchers. Furthermore, it is suitable for the preparation of NMR samples of volatile and semivolatile compounds, especially with sample sizes ranging from several nanograms to several micrograms.