通过降低氯甲酸 9-芴基甲酯的浓度,对低浓度颗粒物中的二甲胺进行定量。

IF 2.7 3区 化学 Q2 CHEMISTRY, ANALYTICAL Analytical Methods Pub Date : 2024-11-22 DOI:10.1039/d4ay00894d
Susana García-Alonso, Francisco Javier Gómez-Moreno, Elisabeth Alonso-Blanco, Rosa María Pérez-Pastor
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引用次数: 0

摘要

本研究介绍了一种采用液相色谱-荧光检测器(LC-FD)对颗粒物(PM)中痕量二甲胺进行定量的改进方法。该方法经过优化,优先考虑了简便性、成本效益和实用性。为确保分析的准确性和可靠性,该方法遵循严格的协议和程序,以尽量减少交叉污染。在一个区域指定了单独的工作空间用于制备对照空白和样品处理,在另一个区域则用于制备标准溶液,从而降低了交叉污染的风险。对不同浓度的 9-芴基甲基氯甲酸酯衍生二甲胺进行了评估。结果表明,浓度为 3 μg mL-1 的二甲胺能有效地衍生出浓度高达 300 ng mL-1 的二甲胺。将衍生试剂的浓度从 2.9 μg mL-1 提高到 7.3 μg mL-1,会导致空白测定中的二甲胺含量略有升高。此外,在制备低浓度标准品时,也发现分析变异系数较高。这凸显了检查潜在污染源的重要性。通过空白分析评估了方法的精确度和定量限,得出的数值分别约为 20% 和 20 纳克/毫升-1,符合环境分析中的色谱测定法。通过分析八个 PM2.5 样品,证明了该方法适用于环境分析。结果发现,甲胺和二甲胺的浓度范围分别为 0.8 至 3 纳克 m-3 和 1.4 至 7.1 纳克 m-3,与文献报道一致。与同时进行的羰基测量结果进行比较后发现,两者的浓度分布相似。这两种类型的分析都可以采用经济实惠的方法进行,即使用较低浓度的衍生试剂事先进行衍生。
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Quantification of dimethylamine in low concentration particulate matter by reducing the concentration of 9-fluorenylmethyl chloroformate.

This study presents a refined method that uses liquid chromatography with a fluorescence detector (LC-FD) to quantify trace amounts of dimethylamine in particulate matter (PM). This method was optimized to prioritize simplicity, cost-effectiveness and practicality. To ensure accurate and reliable analysis, strict protocols and procedures were followed to minimize cross-contamination. Separate workspaces were designated for preparing control blanks and sample treatments in one area and standard solutions in another, thus mitigating the risk of cross-contamination. An evaluation was conducted on different concentrations of 9-fluorenylmethyl chloroformate to derivatize dimethylamine. The results showed that a concentration of 3 μg mL-1 was effective in derivatizing dimethylamine concentrations up to 300 ng mL-1. Increasing the concentration of the derivatization reagent from 2.9 to 7.3 μg mL-1 resulted in slightly elevated dimethylamine levels in blank measurements. Also, during the preparation of standards at low concentrations, high analytical coefficients of variation were observed. This highlights the importance of checking for potential sources of contamination. Method precision and quantification limits were evaluated through blank analysis, yielding values of approximately 20% and 20 ng mL-1, respectively, consistent with chromatographic determination for environmental analysis. The suitability of the method for environmental analysis was demonstrated by analyzing eight PM2.5 samples. The concentrations of methylamine and dimethylamine were found to range from 0.8 to 3 ng m-3 and 1.4 to 7.1 ng m-3, respectively, in accordance with the literature. Comparison with concurrent carbonyl measurements revealed similar concentration profiles. Both types of analyses can be performed using affordable methodologies that involve prior derivatization using a reduced concentration of the derivatization reagent.

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来源期刊
Analytical Methods
Analytical Methods CHEMISTRY, ANALYTICAL-FOOD SCIENCE & TECHNOLOGY
CiteScore
5.10
自引率
3.20%
发文量
569
审稿时长
1.8 months
期刊介绍: Early applied demonstrations of new analytical methods with clear societal impact
期刊最新文献
Quantification of dimethylamine in low concentration particulate matter by reducing the concentration of 9-fluorenylmethyl chloroformate. Synthesis of a fluorescent probe based on rhodol's highly selective recognition of H2S and its application in cells. A novel approach to the extraction and analysis of dioxins and furans sampled onto Amberlite XAD-2 sorbent. Colorimetric aptasensors for sensitive low-density lipoprotein detection based on reduced oxide graphene@molybdenum disulfide-ferrocene nanosheets with peroxidase-like activity. Back cover
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