Highly efficient purification of long-chain alkenones using silver dimercaptotriazine flash chromatography

IF 3.6 2区地球科学 Q1 GEOCHEMISTRY & GEOPHYSICS Chemical Geology Pub Date : 2024-06-22 DOI:10.1016/j.chemgeo.2024.122241

Lu Wang , Yuan Yao , Yongsong Huang , Yinan Zhao , Hai Cheng

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Abstract

Long-chain alkenones (LCAs) are important tools for paleotemperature reconstructions in lacustrine and marine environments. However, some neutral lipid compounds that co-elute with LCAs often occur in natural sediment samples, which seriously interferes with the identification and quantification of the LCAs. In this study, we report a new flash column chromatography based on silver(I)-dimercaptotriazine (Ag-DMT) functionalized silica material (≡Si-DMT-Ag) for purifying and isolating the individual LCAs from complex lake and marine sediment samples. Compared to silver(I)-mercaptopropyl (Ag-MP) functionalized (≡Si-(CH₂)₃-S-Ag) and silver nitrate (SiO₂ + AgNO₃) impregnated silica materials used by previous studies, the Ag-DMT stationary phase displays the best efficiency in removing co-eluting compounds (including wax ester, hopanoid, hopanoic acid, sterane, alkanoic acid, and some unknown compounds) from the LCAs in our study lake and marine sediment samples. The Ag-DMT material also shows its high retention capacity for the LCAs, probably due to a strong interaction of more positively charged silver sites on Ag-DMT with double bonds. Employing the Ag-DMT chromatography, we develop an optimal solvent elution scheme to efficiently isolate the individual LCAs with the same chain length but different numbers of unsaturation for their isotopic analysis in the future. Our study provides a highly effective method for eliminating co-eluting compounds and isolating individual LCAs for paleoclimate studies.

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利用二巯基三嗪银闪蒸色谱法高效纯化长链烯酮类化合物

长链烯酮（LCAs）是重建湖沼和海洋环境古温度的重要工具。然而，在天然沉积物样品中经常会出现一些与长链烯酮共洗脱的中性脂质化合物，这严重干扰了长链烯酮的鉴定和定量。在本研究中，我们报告了一种基于银（I）-二巯基三嗪（Ag-DMT）功能化硅胶材料（≡Si-DMT-Ag）的新型闪柱色谱法，用于纯化和分离复杂湖泊和海洋沉积物样品中的单个 LCAs。与以往研究中使用的银(I)-巯基丙基（Ag-MP）功能化（≡Si-(CH)-S-Ag）和硝酸银（SiO + AgNO）浸渍硅胶材料相比，Ag-DMT 固定相在去除湖泊和海洋沉积物样品中 LCAs 的共沉淀化合物（包括蜡酯、啤酒花酸、啤酒花酸、甾烷、烷酸和一些未知化合物）方面的效率最高。Ag-DMT 材料对 LCA 的保留能力也很高，这可能是由于 Ag-DMT 上带正电荷的银位点与双键之间的相互作用很强。利用 Ag-DMT 色谱法，我们开发出了一种最佳溶剂洗脱方案，可有效地分离出链长相同但不饱和度不同的单个 LCA，以便将来对其进行同位素分析。我们的研究为古气候研究提供了一种消除共沉淀化合物和分离单个 LCA 的高效方法。

本文章由计算机程序翻译，如有差异，请以英文原文为准。

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来源期刊

Chemical Geology 地学-地球化学与地球物理

CiteScore

7.20

自引率

10.30%

发文量

374

审稿时长

3.6 months

期刊介绍： Chemical Geology is an international journal that publishes original research papers on isotopic and elemental geochemistry, geochronology and cosmochemistry. The Journal focuses on chemical processes in igneous, metamorphic, and sedimentary petrology, low- and high-temperature aqueous solutions, biogeochemistry, the environment and cosmochemistry. Papers that are field, experimentally, or computationally based are appropriate if they are of broad international interest. The Journal generally does not publish papers that are primarily of regional or local interest, or which are primarily focused on remediation and applied geochemistry. The Journal also welcomes innovative papers dealing with significant analytical advances that are of wide interest in the community and extend significantly beyond the scope of what would be included in the methods section of a standard research paper.