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Development of a novel comprehensive analytical method for volatile compounds using supercritical fluid chromatography/mass spectrometry with a highly cross-linked styrene divinylbenzene polymer-based column.
Journal of Chromatography A ( IF 4.1 ) Pub Date : 2020-06-22 , DOI: 10.1016/j.chroma.2020.461363
Yuka Fujito 1 , Yoshihiro Hayakawa 2 , Takeshi Bamba 3
Affiliation  

Analytical techniques to determine volatile compounds such as flavor, aroma, and fragrances are in high demand due to their wide range of applications in industry, the chemical properties of them are very diverse. Supercritical fluid chromatography (SFC) is capable of high speed, high peak capacity separation and has a high separation coverage. It is also an advantageous for preparative purifications due to its unique mobile phase conditions. However, there is no column commercially available for SFC that is suitable to comprehensively separate volatile compounds. SFC is limited to the use of silica-based columns due to weak retentions and polymer-based column issues such as pressure, swelling and shrinkage tolerances. This study demonstrated comprehensive analytical method for volatile in SFC using a highly cross-linked styrene divinylbenzene (SDVB) polymer-based column, newly developed for SFC. In this study, 23 typical volatile compounds with a wide variety of chemical properties were selected as model compounds. The newly developed SDVB column showed, compared to conventional silica-based columns (k > 0.3), an excellent overall and substantial improved retentions (k > 1.6) under SFC mobile phase conditions. It was also able to retain esters (hydroxy acetate, pentyl butylate, methyl salicylate) and non-polar terpenes (limonene, pinene) that did not show sufficient retention in any other commercially available silica-based columns. Aldehydes reacting on NH2 column due to Schiff base formation were also successfully eluted. It was confirmed that SDVB column provided comprehensive separation and wide coverage for volatile compounds.



中文翻译:

使用超临界流体色谱/质谱联用高度交联的苯乙烯二乙烯基苯聚合物基色谱柱,开发了一种新颖的挥发性化合物综合分析方法。

由于其在工业中的广泛应用,对确定挥发性化合物(如风味,香气和香料)的分析技术的需求很高,它们的化学性质非常不同。超临界流体色谱(SFC)能够进行高速,高峰容量的分离,并具有很高的分离覆盖率。由于其独特的流动相条件,对于制备型纯化也是有利的。但是,没有可商购的SFC色谱柱适合于全面分离挥发性化合物。由于保留力弱和基于聚合物的色谱柱问题(例如压力,溶胀和收缩容差),SFC仅限于使用基于硅胶的色谱柱。这项研究证明了使用针对SFC新开发的高度交联的苯乙烯二乙烯基苯(SDVB)聚合物基色谱柱对SFC中的挥发物进行综合分析的方法。在这项研究中,选择了23种具有多种化学性质的典型挥发性化合物作为模型化合物。与传统的硅胶色谱柱(k> 0.3)相比,新开发的SDVB色谱柱在SFC流动相条件下具有出色的整体保留率(k> 1.6),并且显着提高了保留率。它还能够保留在任何其他市售的硅胶色谱柱中均未显示出足够保留能力的酯(乙酸羟基酯,丁酸戊酯,水杨酸甲酯)和非极性萜烯(柠檬烯,pin烯)。醛与NH反应 选择了23种具有多种化学性质的典型挥发性化合物作为模型化合物。与传统的硅胶色谱柱(k> 0.3)相比,新开发的SDVB色谱柱在SFC流动相条件下具有出色的整体保留率(k> 1.6),并且显着提高了保留率。它还能够保留在任何其他市售的硅胶色谱柱中均未显示出足够保留能力的酯(乙酸羟基酯,丁酸戊酯,水杨酸甲酯)和非极性萜烯(柠檬烯,pin烯)。醛与NH反应 选择了23种具有多种化学性质的典型挥发性化合物作为模型化合物。与传统的硅胶色谱柱(k> 0.3)相比,新开发的SDVB色谱柱在SFC流动相条件下具有出色的整体保留率(k> 1.6),并且显着提高了保留率。它还能够保留在任何其他市售的硅胶色谱柱中均未显示出足够保留能力的酯(乙酸羟基酯,丁酸戊酯,水杨酸甲酯)和非极性萜烯(柠檬烯,pin烯)。醛与NH反应 它还能够保留在任何其他市售的硅胶色谱柱中均未显示出足够保留能力的酯(乙酸羟基酯,丁酸戊酯,水杨酸甲酯)和非极性萜烯(柠檬烯,pin烯)。醛与NH反应 它还能够保留在任何其他市售的硅胶色谱柱中均未显示出足够保留能力的酯(乙酸羟基酯,丁酸戊酯,水杨酸甲酯)和非极性萜烯(柠檬烯,pin烯)。醛与NH反应由于希夫碱的形成,第二根色谱柱也被成功洗脱。可以肯定的是,SDVB色谱柱可为挥发性化合物提供全面的分离和广泛的覆盖范围。

更新日期:2020-07-05
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