Regueiro Jorge, Llompart Maria, Garcia-Jares Carmen, Cela Rafael
Departamento de Quimica Analitica, Nutricion y Bromatologia, Instituto de Investigacion y Analisis Alimentarios, Universidad de Santiago de Compostela, Santiago de Compostela 15782, Spain.
J Chromatogr A. 2009 Apr 3;1216(14):2816-24. doi: 10.1016/j.chroma.2008.09.110. Epub 2008 Oct 7.
In the present work, a simple and fast methodology has been developed for the analysis of chlorotoluenes in water samples using solid-phase microextraction (SPME) coupled to gas chromatography-tandem mass spectrometry (GC/MS/MS). A multifactorial experimental design strategy was used for studying the influence on extraction yield of factors such as fiber coating, extraction mode, temperature, and addition of sodium chloride. Quantitative recoveries (>/=84%) and satisfactory precision (relative standard deviations (RSD)</=12%) have been obtained. Limits of detection (LODs) in the sub-picogram per litre level from 0.030 to 0.330 were achieved for all analyzed compounds. Linearity was studied in a wide range of concentrations and an analysis of variance with a lack-of-fit test was run to validate the calibration data. Extraction time profiles were also studied, showing that most of chlorotoluenes reached the equilibrium or were close to it. Finally, the applicability of the proposed method has been demonstrated for real samples including river and sewage water samples. Since no matrix effects were observed, quantification could readily be carried out by external calibration with ultrapure water standards.
在本研究中，已开发出一种简单快速的方法，用于分析水样中的氯甲苯，该方法采用固相微萃取（SPME）与气相色谱 - 串联质谱（GC/MS/MS）联用。采用多因素实验设计策略来研究诸如纤维涂层、萃取模式、温度和氯化钠添加量等因素对萃取产率的影响。获得了定量回收率（≥84%）和令人满意的精密度（相对标准偏差（RSD）≤12%）。所有分析化合物的检测限（LOD）在每升亚皮克级水平，范围为0.030至0.330。在很宽的浓度范围内研究了线性关系，并进行了失拟检验的方差分析以验证校准数据。还研究了萃取时间曲线，结果表明大多数氯甲苯达到了平衡或接近平衡。最后，已证明所提出的方法对包括河水和污水水样在内的实际样品具有适用性。由于未观察到基质效应，因此可以通过用超纯水标准品进行外标法轻松进行定量。
