Departamento de Medio Ambiente, INIA, Madrid, Spain.
J Chromatogr A. 2011 Jul 15;1218(28):4291-8. doi: 10.1016/j.chroma.2011.05.030. Epub 2011 May 14.
An analytical method for the determination of UV filters in soil and sediment has been developed and validated considering benzophenones (BP) and salicylates as target analytes. Soil and sediment samples were extracted with ethyl acetate-methanol (90:10, v/v) assisted with sonication, performing a simultaneous clean-up step. Quantification of these compounds was carried out by gas chromatography-mass spectrometry (GC-MS) after derivatization of the extracts with N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA). Recoveries from spiked soil samples ranged from 89.8% to 104.4% and they were between 88.4% and 105.3% for spiked sediment samples. The effect of the residence time and soil moisture content on the recovery of these compounds was also studied. The precision, expressed as relative standard deviation, was in all cases below 6.1% and the limits of detection (S/N=3) varied from 0.07 to 0.10 ng g(-1) and from 0.11 to 0.28 ng g(-1) for soils and sediments, respectively. The validated method was applied to the analysis of five benzophenone and two salicylate UV filters in soil and sediment samples collected in different areas of Spain.
已开发并验证了一种用于测定土壤和沉积物中紫外线滤光剂的分析方法，考虑了苯并二氢吡喃酮（BP）和水杨酸酯作为目标分析物。土壤和沉积物样品用乙酸乙酯-甲醇（90:10，v/v）提取，并用超声辅助提取，同时进行净化步骤。这些化合物的定量通过气相色谱-质谱（GC-MS）进行，在提取物与 N,O-双（三甲基甲硅烷基）三氟乙酰胺（BSTFA）衍生化后进行。从加标土壤样品中的回收率范围为 89.8%至 104.4%，从加标沉积物样品中的回收率范围为 88.4%至 105.3%。还研究了这些化合物在土壤中的停留时间和土壤湿度对回收率的影响。在所有情况下，精密度均表示为相对标准偏差，均低于 6.1%，检出限（S/N=3）分别为 0.07 至 0.10ng g(-1)和 0.11 至 0.28ng g(-1)，用于土壤和沉积物。已验证的方法应用于分析在西班牙不同地区采集的土壤和沉积物样品中的五种苯并二氢吡喃酮和两种水杨酸酯紫外线滤光剂。
