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首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >Improving the productivity of a multidimensional chromatographic preparative system by collecting pure chemicals after each of three chromatographic dimensions
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Improving the productivity of a multidimensional chromatographic preparative system by collecting pure chemicals after each of three chromatographic dimensions

机译:通过在三个色谱维之后分别收集纯净化学物质,提高多维色谱制备系统的生产率

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摘要

The enhanced sample collection capability of a heart-cutting three-dimensional GC-prep system is reported. In its original configuration, a highly pure component can be usually collected after the last (3D) column outlet by means of a dedicated preparative station. The latter is located after the last chromatographic column, and this poses the requirement for multiple heart cuts even for those components showing satisfactory degree of purity after the first (or second) separation dimension. The feasibility to collect pure components after each chromatographic dimension is here described, employing a three dimension MDGC system equipped with high-temperature valves, located inside the first and second GC ovens, with the aim to improve the productivity of the collection procedure. In addition to a commercial preparative collector located at the 3D outlet, two laboratory-made collection systems were applied in the first and second dimension, reached by the effluent to be collected trough a high-temperature valve switching the heart-cut fraction between either the detector (FID), or the collector. Highly pure sesquiterpene components were collected, namely: patchouli alcohol after the first column [poly(5% diphenyl/95% dimethylsiloxane)], alpha-bulnesene after a second column coated with high molecular weight polyethylene glycol, and a-guaiene after an ionic-liquid based column (SLB-IL60), used as the third dimension. Purity levels ranging from 85 to 95% were achieved with an average collection recovery of 90% (n = 5). The following average amounts were collected per run: 160 mu g for alpha-guaiene, 295 mu g for alpha-bulnesene, and 496 mu g for patchouli alcohol. (C) 2016 Elsevier B.V. All rights reserved.
机译:据报导,心脏切割三维气相色谱制备系统具有增强的样品收集能力。在其原始配置中,通常可以通过专用的制备工作站在最后一个(3D)色谱柱出口之后收集高纯度组分。后者位于最后一个色谱柱之后,即使在第一(或第二)分离尺寸后显示出令人满意的纯度的那些成分,也要求进行多次心脏切割。在此描述了在每个色谱图尺寸后收集纯组分的可行性,该方法采用了配备有高温阀的三维MDGC系统,该系统位于第一和第二GC柱箱内,目的是提高收集程序的生产率。除了位于3D出口处的商用制备性收集器外,在第一维和第二维上应用了两个实验室制造的收集系统,废水通过高温阀到达收集的流出物,高温阀在两个检测器(FID)或收集器。收集高纯度倍半萜烯成分,即:第一列后的广patch香醇[聚(5%二苯基/ 95%二甲基硅氧烷)],第二列经高分子量聚乙二醇包被的α-芳烃和离子后的α-愈创木酚-基于液体的色谱柱(SLB-IL60),用作第三维。纯度达到85%至95%,平均回收率达到90%(n = 5)。每次运行收集的平均量如下:α-番石榴烯为160克,α-戊烯为295克,广patch香醇为496克。 (C)2016 Elsevier B.V.保留所有权利。

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