Université de Lyon - Institut des Sciences Analytiques, Département Service Central d'Analyse - UMR 5280 CNRS, Université Lyon1, ENS-Lyon - 5 rue de la Doua, 69100 Villeurbanne, France.
Talanta. 2012 May 15;93:336-44. doi: 10.1016/j.talanta.2012.02.048. Epub 2012 Mar 3.
A novel multiresidue method was developed for the simultaneous analysis of 34 organochlorines, including chlorobenzenes, chlorophenols, chlorinated hydrocarbons and chlorinated olefins, in soil by GC-MS, using a QuEChERS-based extraction. The conventional QuEChERS method was optimised and, for the first time, the use of a non miscible-water solvent was required. The method was compared to ASE extraction, versatile technique widely used for the soils' extraction and QuEChERS-based method was shown to be the most efficient in terms of recoveries, simplicity and rapidity. For ASE, recoveries between 42% and 85% were obtained for the majority of the compounds. However, due to the high pressure, all volatile compounds were lost. In opposite, QuEChERS extraction allowed detection and quantification of all the compounds with recoveries between 60% and 100%. Moreover, no additional clean up by dispersive SPE on PSA was necessary, which allowed reducing the cost of the analysis. Performance of the method was assessed. The method was linear over the range of concentration of 10-5000 μg kg(-1). Precision, expressed as intra-day precision and inter-day variation was verified at three concentrations. Limits of detection were from 2 to 50 μg kg(-1) and limits of quantification from 7 to 170 μg kg(-1) for the majority of the compounds (chlorobenzenes and chlorinated hydrocarbons and olefins), except for chlorophenols. The method was further applied to different soils coming from a contaminated industrial site, where a new environmental remediation process, using phytoremediation, was tested. The results showed that the method could be applied to any kind of soils (mineral or organic) and was appropriate to very volatile compounds which were not available with conventional technique.
一种新的多残留方法已经被开发出来,用于通过 GC-MS 同时分析土壤中的 34 种有机氯农药,包括氯苯、氯酚、氯化烃和氯化烯烃,采用 QuEChERS 萃取法。对常规 QuEChERS 方法进行了优化,并首次需要使用不混溶的水溶剂。该方法与 ASE 萃取进行了比较,ASE 是一种广泛用于土壤提取的通用技术,QuEChERS 方法在回收率、简单性和快速性方面表现出最高的效率。对于 ASE,大多数化合物的回收率在 42%至 85%之间。然而,由于高压,所有挥发性化合物都丢失了。相反,QuEChERS 萃取允许检测和定量所有化合物,回收率在 60%至 100%之间。此外,不需要通过 PSA 上的分散 SPE 进行额外的净化,这降低了分析成本。评估了该方法的性能。该方法在浓度为 10-5000 μg kg(-1)的范围内呈线性。在三个浓度下验证了日内精密度和日间变异的精密度。大多数化合物(氯苯和氯化烃和烯烃)的检测限为 2 至 50 μg kg(-1),定量限为 7 至 170 μg kg(-1),除了氯酚。该方法进一步应用于来自污染工业场地的不同土壤,在该场地中测试了一种使用植物修复的新环境修复过程。结果表明,该方法可适用于任何类型的土壤(矿物质或有机),并且适用于常规技术无法获得的非常挥发性化合物。