首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >Determination of parabens in house dust by pressurised hot water extraction followed by stir bar sorptive extraction and thermal desorption-gas chromatography-mass spectrometry
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Determination of parabens in house dust by pressurised hot water extraction followed by stir bar sorptive extraction and thermal desorption-gas chromatography-mass spectrometry

机译:加压热水萃取-搅拌棒吸附萃取-热脱附-气相色谱-质谱法测定室内灰尘中的对羟基苯甲酸酯

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This study describes the development of a new method for determining p-hydroxybenzoic esters (parabens) in house dust. This optimised method was based on the pressurised hot water extraction (PHWE) of house dust, followed by the acetylation of the extracted parabens, stir bar sorptive extraction (SBSE) with a polydimethylsiloxane stir bar, and finally analysis using thermal desorption-gas chromatography-mass spectrometry (TD-GC-MS). The combination of SBSE and PHWE allows the analytes to be preconcentrated and extracted from the aqueous extract in a single step with minimal manipulation of the sample. Furthermore the in situ acetylation of parabens prior to SBSE improved their extraction efficiency and their GC-MS signal. The method showed recoveries of between 40 and 80%, good linearity, repeatability and reproducibility (<10% RSD, at 100ngg~(-1), n=5), low limits of detection (from 1.0ngg~(-1) for propyl paraben to 2.1ngg~(-1) for methyl paraben) and quantification (from 3.3ngg~(-1) for propyl paraben to 8.5ngg~(-1) for methyl paraben). The proposed method was applied to the analysis of house dust samples. All the target parabens were found in the samples. Methyl and propyl parabens were the most abundant, with concentrations up to 2440ngg~(-1) and 910ngg~(-1), respectively. The high levels of parabens found in the samples confirm the importance of determining organic contaminants in indoor environments.
机译:这项研究描述了一种测定室内灰尘中对羟基苯甲酸酯(对羟基苯甲酸酯)的新方法的开发。此优化方法基于以下条件:对室内灰尘进行加压热水萃取(PHWE),然后对萃取的对羟基苯甲酸酯进行乙酰化,然后使用聚二甲基硅氧烷搅拌棒进行搅拌棒吸附萃取(SBSE),最后使用热脱附气相色谱分析质谱(TD-GC-MS)。 SBSE和PHWE的组合使分析物可以在一个步骤中以最少的样品操作就可以从水提取物中进行预浓缩和提取。此外,SBSE之前对羟基苯甲酸酯的原位乙酰化提高了其提取效率和GC-MS信号。该方法的回收率在40%至80%之间,线性度,重复性和重现性好(相对标准偏差<10%,在100ngg〜(-1),n = 5),检测下限低(从1.0ngg〜(-1)对羟基苯甲酸丙酯对羟基苯甲酸甲酯为2.1ngg〜(-1))和定量(对羟基苯甲酸丙酯为3.3ngg〜(-1)对羟基苯甲酸甲酯为8.5ngg〜(-1))。该方法被应用于室内灰尘样品的分析。在样品中发现了所有目标对羟基苯甲酸酯。对羟基苯甲酸甲酯和对羟基苯甲酸丙酯含量最高,分别达到2440ngg〜(-1)和910ngg〜(-1)。样品中发现的高水平的对羟基苯甲酸酯证实了确定室内环境中有机污染物的重要性。

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