Departamento de Química Analítica, Nutrición y Bromatología, Instituto de Investigación y Análisis Alimentario, Universidad de Santiago de Compostela, Santiago de Compostela 15782, Spain.
Anal Bioanal Chem. 2010 Nov;398(5):2289-97. doi: 10.1007/s00216-010-4136-3. Epub 2010 Aug 31.
An expeditious method for the determination of triclosan (TCS) and methyl triclosan (MTCS) in sludge and sediment samples is presented. Extraction and cleanup steps were integrated in the same process using matrix solid-phase dispersion as sample preparation technique. Effects of different variables on the efficiency and the selectivity of the sample preparation process are discussed. Under final working conditions, samples (0.5 g) were dispersed with diatomaceous earth (1 g) and transferred to a polypropylene syringe containing 2 g of silica impregnated with sulphuric acid (15%, w:w). Analytes were recovered with 10 mL of dichloromethane. After solvent exchange to ethyl acetate, TCS was converted into the tert-butyldimethylsilyl derivative, and the extract was analysed by gas chromatography-mass spectrometry, without any additional cleanup. Obtained recoveries, for sludge and sediment samples spiked at different concentration levels, ranged from 86% to 113%, with associated standard deviations between 2 and 13%. Limits of quantification of the global method were 6 and 7 ng g(-1) for MTCS and TCS, respectively. Both compounds were detected in all the processed sludge samples with maximum concentrations of 191 ng g(-1) (MTCS) and 2,640 ng g(-1) (TCS). The parent bactericide was also found in some sediment samples at concentrations up to 200 ng g(-1).
一种快速测定污泥和沉积物样品中三氯生（TCS）和甲基三氯生（MTCS）的方法。提取和净化步骤在同一过程中集成，使用基质固相分散作为样品制备技术。讨论了不同变量对样品制备过程效率和选择性的影响。在最终工作条件下，将（0.5 g）样品与硅藻土（1 g）分散，并转移到含有硫酸浸渍硅胶（15%，w/w）的 2 g 聚丙烯注射器中。用 10 mL 二氯甲烷回收分析物。在溶剂交换为乙酸乙酯后，TCS 被转化为叔丁基二甲基甲硅烷基衍生物，并用气相色谱-质谱法分析提取物，无需进行任何额外的净化。在不同浓度水平下对污泥和沉积物样品进行加标回收，回收率范围为 86%至 113%，相对标准偏差在 2%至 13%之间。总方法的定量限分别为 MTCS 和 TCS 的 6 和 7 ng g(-1)。在所处理的所有污泥样品中均检测到这两种化合物，其浓度最高分别为 191 ng g(-1)（MTCS）和 2,640 ng g(-1)（TCS）。在一些沉积物样品中也发现了母体杀菌剂，浓度高达 200 ng g(-1)。
