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首页> 外文期刊>Journal of Environmental Science and Health. A, Toxic/Hazardous Substances & Environmental Engineering >Evaluation of nitrobenzenes and chlorobenzenes levels in samples of sediments from Italy: A rapid and simple method by automatic extractor and GC/MS ion trap
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Evaluation of nitrobenzenes and chlorobenzenes levels in samples of sediments from Italy: A rapid and simple method by automatic extractor and GC/MS ion trap

机译：评估意大利沉积物中样品中的硝基苯和氯苯含量：通过自动萃取器和GC / MS离子阱的快速简便方法

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Ninety-six marine sediment samples from an Italian harbour were analysed by GC/MS ion trap for the residues of nitrobenzenes and chlorobenzenes. The significance of these compounds in the investigated matrix was discussed. In order to determine the simultaneous presence of chlorobenzenes and nitrobenzenes in marine sediments, a simple extraction method by an automatic extraction system was developed. The use of an automatic extractor unit allows the extraction of the analytes of interest with no waste of volatile compounds, since small volumes of solvent are required. This also results in a reduction of the analysis time, compared with traditional extraction techniques such as extraction by Soxhlet. The samples under investigation were mixed with anhydrous sodium sulphate to obtain a free-flowing powder and quantitatively transferred into extraction thimbles. The thimbles were then introduced into the automatic extractor unit by solvent and extracted with 70 mL of acetone/hexane (1:1, v/v). The extract was analysed directly by GC/MS ion trap in EI mode. A VF5 ms low bleeding capillary column was used to separate the compounds of interest. Recovery rates were determined at two spiking levels, one ranging from 1.0 to 5.0 mg/kg, the other from 10 to 50 mg/kg. Six replicates were analysed for each fortification level. Mean recoveries proved to range from 60.6 to 125.1% in either case. The precision of the method was expressed as relative standard deviation (RSD%), which turned out to be in the range 5.2-15.0%. The determination limits ranged from 0.01 mg/kg to 1.0 mg/kg, when approximately 10 g (dry weight) samples were considered. The linearity (r~2 > 0.99) and the limit of detection were also studied.
机译：通过GC / MS离子阱分析了来自意大利港口的96个海洋沉积物样品中的硝基苯和氯苯残留物。讨论了这些化合物在所研究基质中的重要性。为了确定海洋沉积物中同时存在氯苯和硝基苯，开发了一种利用自动提取系统的简单提取方法。由于需要少量溶剂，因此使用自动提取器单元可以在不浪费挥发性化合物的情况下提取目标分析物。与传统的提取技术（如索氏提取）相比，这也减少了分析时间。将要研究的样品与无水硫酸钠混合以获得自由流动的粉末，然后定量转移到萃取套管中。然后通过溶剂将顶针引入自动萃取器单元，并用70 mL丙酮/己烷（1：1，v / v）萃取。提取物通过EI模式的GC / MS离子阱直接分析。使用VF5 ms低出血毛细管色谱柱分离目标化合物。确定了两种加标水平的回收率，一种在1.0至5.0 mg / kg的范围内，另一种在10至50 mg / kg的范围内。对于每个设防级别，分析了六个重复样本。在这两种情况下，平均回收率均证明为60.6％至125.1％。该方法的精度表示为相对标准偏差（RSD％），结果在5.2-15.0％的范围内。当考虑大约10 g（干重）样品时，测定极限范围为0.01 mg / kg至1.0 mg / kg。还研究了线性度（r〜2> 0.99）和检出限。

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