Miniaturised pressurised liquid extraction of polycyclic aromatic hydrocarbons from soil and sediment with subsequent large-volume injection-gas chromatography.
Miniaturised pressurised liquid extraction of polycyclic aromatic hydrocarbons from soil and sediment with subsequent large-volume injection-gas chromatography.
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从土壤和沉积物中微型加压液体萃取多环芳烃，并随后进行大体积注射气相色谱分析。
DOI：
10.1016/s0021-9673(00)00652-x
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发表时间：
2000
期刊：
影响因子：
--
通讯作者：
U. Brinkman
中科院分区：
文献类型：
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作者：
L. Ramos;J. J. Vreuls;U. Brinkman
分析物提取是开发在线或在线制备（半）固体环境样品程序时的主要限制。加压液体萃取（PLE）是一种不依赖于分析物和基质的技术，它比耗时的经典程序提供更清洁的萃取物。在这项研究中，在不锈钢池中进行，并与随后的大体积注射（LVI）-GC-MS相结合的实用性进行了研究。以土壤和沉积物中多环芳烃（PAHs）的测定为例进行了验证。影响PLE效率的变量，如萃取溶剂的压力和温度以及总溶剂体积，进行了研究。选择甲苯作为浸提溶剂，总溶剂体积为100 μl，用于50 mg样品的10 min静态-动态PLE。不需要对样品浸提液进行额外的清洁或过滤。真实的土壤样品中13种比茚并[1，2，3-cd]芘挥发性更强的多环芳烃的LVI-GC-MS检测限均低于9 ng/g土壤，PLE + LVI-GC-MS分析内源性多环芳烃的重复性优于15%。比较PLE和索氏提取或液体分配提取法分析未加标样品的结果表明，PLE的效率与其他两种提取方法相同或更好。
Analyte extraction is the main limitation when developing at-line, or on-line, procedures for the preparation of (semi)solid environmental samples. Pressurised liquid extraction (PLE) is an analyte- and matrix-independent technique which provides cleaner extracts than the time-consuming classical procedures. In the study, the practicality of miniaturised PLE performed in a stainless-steel cell, and combined with subsequent large-volume injection (LVI)–GC–MS was studied. As an example, the new system was applied to the determination of polycyclic aromatic hydrocarbons (PAHs) in soils and a sediment. Variables affecting the PLE efficiency, such as pressure and temperature of the extraction solvent and total solvent volume, were studied. Toluene was selected as extraction solvent and a total solvent volume of 100 μl was used for the 10 min static-dynamic PLE of 50-mg samples. Additional clean-up or filtration of the sample extracts was not required. Detection limits using LVI–GC–MS were below 9 ng/g soil for the 13 PAHs more volatile than indeno[1,2,3-cd]pyrene in real soil samples and the repeatability of the complete PLE plus LVI–GC–MS method for the analysis of the endogenous PAH was better than 15%. Comparison of PLE and Soxhlet or liquid-partitioning extraction results for the analysis of non-spiked samples showed that the efficiency of PLE is the same or better than for the other two extraction methods assayed.