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Quantification of lipid biomarkers in sedimentary contexts: comparing different calibration methods
Organic Geochemistry ( IF 2.6 ) Pub Date : 2018-11-01 , DOI: 10.1016/j.orggeochem.2018.07.009
Antonio V. Herrera-Herrera , Carolina Mallol

Abstract The analysis of lipid biomarkers has gained increasing importance within environmental and archaeological fields because biomarkers are representative of particular plant and animal sources. Accurate quantification of such compounds is essential to obtaining significant information. In this paper, accuracy in the quantification of n-alkanes (as model compounds) in sedimentary contexts was studied using three different approaches: proportions of chromatographic peak areas with regards to an internal standard, instrumental calibration, and matrix-matched calibration. Alkanes were extracted by ultrasonic assisted solid-liquid extraction and analyzed by gas chromatography coupled to mass spectrometry. Instrumental calibration curves were obtained with determination coefficients (R2) higher than 0.9900. The matrix effect was studied (in the range between −100% and 140%) and matrix-matched calibration curves with R2 above 0.9904 were obtained. Matrix matched calibration provided the best results (percentages in the range 10–130%) when compared with instrumental calibration (1–150%) and no calibration (2–274%). Four sediment samples from an archaeological Neanderthal site were analyzed with the three quantification methods and Student’s t-test demonstrated that the results obtained were significantly different: concentrations were non-uniformly under- or overestimated and the highest peak and the alkane profile varied with the different methods. According to these data, matrix-matched calibration should be the preferred method for quantification since then results are more accurate with only a small amount of extra work. This method requires that control sediment samples are collected at the site under consideration.

中文翻译:

沉积环境中脂质生物标志物的量化:比较不同的校准方法

摘要 脂质生物标志物的分析在环境和考古领域变得越来越重要,因为生物标志物代表特定的植物和动物来源。此类化合物的准确定量对于获得重要信息至关重要。在本文中,使用三种不同的方法研究了沉积环境中正构烷烃(作为模型化合物)定量的准确性:色谱峰面积相对于内标的比例、仪器校准和基质匹配校准。烷烃通过超声辅助固液萃取进行萃取,并通过气相色谱与质谱联用进行分析。仪器校准曲线的测定系数 (R2) 高于 0.9900。研究了基质效应(在 -100% 和 140% 之间的范围内)并获得了 R2 高于 0.9904 的基质匹配校准曲线。与仪器校准 (1-150%) 和无校准 (2-274%) 相比,基质匹配校准提供了最佳结果(百分比范围为 10-130%)。使用三种量化方法分析了考古尼安德特人遗址的四个沉积物样品,学生 t 检验表明获得的结果有显着差异:浓度不均匀地低估或高估,最高峰和烷烃分布随不同的方法。根据这些数据,基质匹配校准应该是首选的定量方法,因为这样只需少量额外工作即可获得更准确的结果。
更新日期:2018-11-01
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