Department of Analytical Chemistry, University of Almeria, Carretera Sacramento s/n, E-04071 Almeria, Spain.
Talanta. 2011 Oct 15;85(5):2397-404. doi: 10.1016/j.talanta.2011.07.081. Epub 2011 Jul 29.
An analytical methodology has been developed for the simultaneous extraction of 13 phenolic compounds, including chlorophenols (CPs), nitrophenols (NTPs), cresols and alkylphenols (APs) in different types of wastewater (WW) effluents. A solid-phase extraction (SPE) method has been optimized prior to the determination by gas chromatography coupled to triple quadrupole tandem mass spectrometry (GC-QqQ-MS/MS). Due to the complexity of the matrix, a comparison study of matrix-matched-calibration (MMC) and standard addition calibration (SAC) was carried out for quantification purposes. The optimized procedure was validated using the SAC approach since it provided the most adequate quantification results (in terms of recovery and precision values). Recoveries were in the range 60-135% (0.5 μg L(-1)), 70-115% (1 μg L(-1)), and 78-120% (5 μg L(-1)), with precision values (expressed as relative standard deviation, RSD) ≤ 30% (except for 2-nitrophenol) involving intra-day and inter-day precision studies. Limits of detection (LODs) and quantification (LOQs) were also evaluated, and LOQs ranged from 0.03 μg L(-1) to 2.5 μg L(-1). The proposed method was applied to the analysis of 8 real WW effluent samples, finding some phenolic compounds (e.g. 2-chlorophenol, 2,4,6-trichlorophenol and 4-tert-octylphenol) at concentrations higher than the established LOQs.
已经开发出一种分析方法，用于同时提取 13 种酚类化合物，包括不同类型废水（WW）废水中的氯酚（CPs）、硝基酚（NTPs）、甲酚和烷基酚（APs）。在通过气相色谱与三重四极杆串联质谱（GC-QqQ-MS/MS）进行测定之前，已经优化了固相萃取（SPE）方法。由于基质的复杂性，进行了基质匹配校准（MMC）和标准添加校准（SAC）的比较研究，以进行定量目的。由于最适合定量结果（回收率和精密度值），因此使用 SAC 方法优化了程序。回收率在 60-135%（0.5μg L（-1））、70-115%（1μg L（-1））和 78-120%（5μg L（-1））范围内，精密度值（表示为相对标准偏差，RSD）≤30%（2-硝基酚除外），涉及日内和日间精密度研究。还评估了检测限（LODs）和定量限（LOQs），LOQs 范围为 0.03μg L（-1）至 2.5μg L（-1）。该方法应用于 8 个实际 WW 废水样品的分析，发现一些酚类化合物（例如 2-氯苯酚、2,4,6-三氯苯酚和 4-叔辛基苯酚）的浓度高于规定的 LOQs。
