Department of Analytical Chemistry, University of Almeria, Spain.
J Chromatogr A. 2010 Sep 3;1217(36):5724-31. doi: 10.1016/j.chroma.2010.07.004. Epub 2010 Aug 3.
Due to the different physico-chemical properties of phenols, the development of a methodology for the simultaneous extraction and determination of phenolic compounds belonging to several families, such as chlorophenols (CPs), alkylphenols (APs), nitrophenols (NTPs) and cresols is difficult. This study shows the development and validation of a method for the analysis of 13 phenolic compounds (including CPs, APs, NTPs and cresols) in agricultural soils. For this purpose, a quick, easy, cheap, effective, rugged and safe (QuEChERS)-based procedure was developed, validated and applied to the analysis of real samples. A derivatization step prior to the final determination by gas chromatography (GC) coupled to a triple quadrupole analyzer operating in tandem mass spectrometry (QqQ-MS/MS) was performed by using acetic acid anhydride (AAA) and pyridine (Py). The optimized procedure was validated, obtaining average extraction recoveries in the range 69-103% (10microgkg(-1)), 65-98% (50microgkg(-1)), 76-112% (100microgkg(-1)) and 76-112% (300microgkg(-1)), with precision values (expressed as relative standard deviation, RSD)< or =22% (except for 4-chlorophenol) involving intra-day and inter-day studies. Furthermore, 15 real soil samples were analyzed by the proposed method in order to assess its applicability. Some phenolic compounds (e.g. 2,4,6-trichlorophenol or 4-tert-octylphenol) were found in the samples at trace levels (<10microgkg(-1)).
由于酚类物质具有不同的物理化学性质,因此开发一种同时提取和测定属于几个家族的酚类化合物(如氯酚、烷基酚、硝基酚和甲酚)的方法具有一定的难度。本研究展示了一种用于分析农业土壤中 13 种酚类化合物(包括氯酚、烷基酚、硝基酚和甲酚)的方法的开发和验证。为此,开发、验证了一种基于 QuEChERS 的快速、简便、廉价、有效、耐用和安全(QuEChERS)的方法,并将其应用于实际样品的分析。在最终通过气相色谱(GC)与串联质谱(QqQ-MS/MS)联用进行测定之前,通过使用乙酸酐(AAA)和吡啶(Py)进行衍生化步骤。对优化后的方法进行了验证,得到了平均提取回收率在 10microgkg(-1)范围内为 69-103%、50microgkg(-1)范围内为 65-98%、100microgkg(-1)范围内为 76-112%和 300microgkg(-1)范围内为 76-112%,精密度值(表示为相对标准偏差,RSD)<或=22%(除 4-氯酚外),涉及日内和日间研究。此外,还通过所提出的方法分析了 15 个实际土壤样品,以评估其适用性。在样品中发现了一些酚类化合物(如 2,4,6-三氯苯酚或 4-叔辛基酚),其含量处于痕量水平(<10microgkg(-1))。