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通过加压液体萃取和热解气相色谱法对环境样品中的微塑料进行定量分析。

Quantification of microplastics in environmental samples via pressurized liquid extraction and pyrolysis-gas chromatography.

机构信息

German Federal Institute of Hydrology, Am Mainzer Tor 1, 56068, Koblenz, Germany.

Institute of Integrated Natural Sciences, University Koblenz-Landau, Universitätsstr. 1, 56070, Koblenz, Germany.

出版信息

Anal Bioanal Chem. 2019 Oct;411(26):6959-6968. doi: 10.1007/s00216-019-02066-9. Epub 2019 Aug 30.

Abstract

The quantification of microplastics (MP) in environmental samples is currently a challenging task. To enable low quantification limits, an analytical method has been developed combining pressurized liquid extraction (PLE) and pyrolysis GC-MS. The automated extraction includes a pre-extraction step via methanol followed by a subsequent PLE using tetrahydrofuran. For the most frequently used synthetic polymers polyethylene (PE), polypropylene (PP), and polystyrene (PS), limits of quantification were achieved down to 0.007 mg/g. Recoveries above 80% were attained for solid matrices such as soil and sediments. The developed method was applied for MP quantification in environmental samples such as sediment, suspended matter, soil, and sewage sludge. In all these matrices, PE and PP were detected with concentrations ranging from 0.03 to 3.3 mg/g. In sewage sludge samples, all three polymers were present with concentration levels ranging between 0.08 ± 0.02 mg/g (PP) and 3.3 ± 0.3 mg/g (PE). However, especially for solid samples, the analysis of triplicates revealed elevated statistical uncertainties due to the inhomogeneous distribution of MP particles. Thus, care has to be taken when milling and homogenizing the samples due to the formation of agglomerates. Graphical abstract.

摘要

目前,量化环境样品中的微塑料(MP)是一项具有挑战性的任务。为了实现低定量限,开发了一种结合加压液体萃取(PLE)和热解气相色谱-质谱(GC-MS)的分析方法。自动提取包括甲醇的预提取步骤,随后使用四氢呋喃进行 PLE。对于最常用的合成聚合物聚乙烯(PE)、聚丙烯(PP)和聚苯乙烯(PS),达到了低至 0.007mg/g 的定量限。对于土壤和沉积物等固体基质,回收率超过 80%。所开发的方法用于环境样品(如沉积物、悬浮物、土壤和污水污泥)中的 MP 定量。在所有这些基质中,均检测到 PE 和 PP,浓度范围为 0.03 至 3.3mg/g。在污水污泥样品中,所有三种聚合物均存在,浓度范围在 0.08±0.02mg/g(PP)和 3.3±0.3mg/g(PE)之间。然而,特别是对于固体样品,由于 MP 颗粒的不均匀分布,三倍分析显示出较高的统计不确定性。因此,在研磨和均化样品时应小心,因为会形成团聚体。

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