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Solid-phase microextraction for the determination of iron organic compounds in seawaters and soils by gas chromatography coupled to microwave-induced plasma with atomic emission detection spectrometry
Microchemical Journal ( IF 4.8 ) Pub Date : 2020-05-01 , DOI: 10.1016/j.microc.2020.104630
Rosa Peñalver , Natalia Campillo , Ignacio López-García , Manuel Hernández-Córdoba

Abstract A rapid solvent-free method for determining ferrocene and five derivatives (1,1´-dimethylferrocene, ferrocenecarboxaldehyde, acetylferrocene, ferroceneacetonitrile and benzoylferrocene) in seawaters and soils using direct immersion solid-phase microextraction (DI-SPME) and gas chromatography coupled to microwave-induced plasma with atomic emission detection (GC-MIP-AED) is developed. The bonded divinylbenzene/Carboxen/polydimethylsiloxane commercial fiber provided good extraction efficiency in the DI mode for all the compounds, applying a fiber time exposure of 15 min at ambient temperature. The analytes were previously isolated from the soil matrices (0.2 g) by ultrasound-assisted extraction using 7 mL of 0.1 M acetate/acetic buffer solution. The absence of a matrix effect was confirmed in the case of seawaters, which permitted calibration against aqueous standards. However, the standard additions method was required for soil analysis. Detection limits (DLs) were in the 3–110 pg mL−1 and 0.9–4 ng g − 1 for seawater and soils, respectively. Analysis of the different samples using the proposed DI-SPME-GC-AED method only provided an analytical signal for ferrocene in one seawater sample at a concentration near its DL (3 pg mL−1).

中文翻译:

气相色谱-微波诱导等离子体原子发射检测光谱法测定海水和土壤中铁有机化合物的固相微萃取

摘要 一种使用直接浸入固相微萃取 (DI-SPME) 和气相色谱法测定海水和土壤中二茂铁和五种衍生物(1,1´-二甲基二茂铁、二茂铁甲醛、乙酰二茂铁、二茂铁乙腈和苯甲酰二茂铁)的快速无溶剂方法开发了具有原子发射检测功能的微波诱导等离子体 (GC-MIP-AED)。键合的二乙烯基苯/羧基/聚二甲基硅氧烷商用纤维在 DI 模式下为所有化合物提供了良好的提取效率,在环境温度下应用 15 分钟的纤维时间暴露。使用 7 mL 0.1 M 醋酸盐/醋酸缓冲溶液,通过超声波辅助萃取,预先从土壤基质 (0.2 g) 中分离出分析物。在海水的情况下证实不存在基质效应,这允许针对水性标准进行校准。然而,土壤分析需要标准添加法。海水和土壤的检测限 (DL) 分别为 3-110 pg mL-1 和 0.9-4 ng g-1。使用建议的 DI-SPME-GC-AED 方法对不同样品的分析仅提供了一个海水样品中浓度接近其 DL (3 pg mL-1) 的二茂铁的分析信号。
更新日期:2020-05-01
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