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首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >An efficient approach to eliminate steryl ethers and miscellaneous esters/ketones for gas chromatographic analysis of alkenones and alkenoates
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An efficient approach to eliminate steryl ethers and miscellaneous esters/ketones for gas chromatographic analysis of alkenones and alkenoates

机译：一种有效的方法，消除碱和链烯酸盐气相色谱分析的斯蒂尔醚和杂项酯/酮

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摘要

Long-chain alkenones (LCAs) and alkenoates (LCEs) are highly valuable biomarkers for paleotemperature reconstructions. A major problem, however, for accurate quantification of these compounds using gas chromatography (GC) is co-elution with steryl ethers, wax esters, saturated ketones and other numerous mid-polarity compounds frequently encountered in marginal marine and lake sediments. Co-elution during GC separation is prevalent, particularly if the full homologous series of alkenones and alkenoates are to be analyzed. Taking advantage of the presence of two or more double bonds in LCAs and LCEs, the conventional silica gel impregnated with silver nitrate has previously been used to remove co-eluting compounds for LCAs. However, this conventional argentation chromatography is hampered by the extreme instability of silver nitrate, poor reproducibility, low recovery and short lifetime. Here we demonstrate a highly efficient flash chromatographic approach based on silver thiolate chromatographic material (AgTCM) that overcomes the shortcomings of the traditional argentation chromatography and allows repeated sample preparation (up to 62 samples in one test) with little loss in separation efficiency. AgTCM selectively extracts LCAs and LCEs and effectively eliminates co-eluting compounds including steryl ethers and wax esters for the subsequent gas chromatography (GC) analysis. This new method, therefore, allows low-cost and high-throughput sample preparation for comprehensive quantification of the full homologous series of LCAs and LCEs in marine and lake sediments. (C) 2019 Elsevier B.V. All rights reserved.
机译：长链链烯酮（LCA）和链烯酸盐（LCE）是古温度重建的高价值生物标志物。然而，对于使用气相色谱（GC）准确定量这些化合物的主要问题是用Steryl醚，蜡酯，饱和酮和在边缘海洋和湖泊沉积物中经常遇到的其他许多中间极性化合物共洗涤。在GC分离期间共洗涤普遍，特别是如果要分析全同源的链烯酮和链烯醇酸盐。利用LCAs和LCE中的两个或更多个双键的存在，浸渍有硝酸银浸渍的常规硅胶预先用于去除用于LCA的共洗脱化合物。然而，这种常规的本发明化学色谱由硝酸银银，再现性差，恢复低，寿命短的极端不稳定性受到阻碍。在这里，我们证明了一种基于银硫醇的闪光色谱法（AGTCM）的高效闪光色谱方法，该方法克服了传统的本发明化学色谱的缺点，并允许重复的样品制备（在一次测试中最多62个样品），分离效率几乎没有损失。 AGTCM选择性地提取LCA和LCE，并有效地消除了用于随后的气相色谱（GC）分析的Cheryl醚和蜡酯的共洗脱化合物。因此，这种新方法允许低成本和高通量的样品准备进行综合量化船舶和湖泊沉积物的全同源系列LCAS和LCE。 （c）2019 Elsevier B.v.保留所有权利。

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