Laboratories Division, BRGM, 3 avenue Claude Guillemin, BP6009, 45060, Orléans Cedex, France,
Anal Bioanal Chem. 2014 Feb;406(4):1073-80. doi: 10.1007/s00216-013-7160-2. Epub 2013 Jul 9.
An analytic method was developed and validated for the analysis of chlordecone in the three main types of French West Indies soils: Ferralsol, Andosol and Nitisol with and without the addition of Daramend® and compost amendment used in a remediation process. The method consists in analysis by gas chromatography coupled with triple quadrupole mass spectrometry after pressurised liquid extraction. The high natural content of organic matter in the soils coupled with the additional exogenous organic matter from the amendments tested lead to a complex extract. Trans-nonachlor was used as surrogate to correct the results for extraction efficiency, and (13)C chlordecone was added as internal standard to mimic as closely as possible the behaviour of chlordecone and suppress possible side effects during its analysis. The key parameters of the method (linearity, repeatability, interday precision, specificity, extraction efficiency and limit of quantification) were validated in accordance with the NF T 90-210 standard method. The limit of quantification is 0.03 mg/kg. Uncertainty (k = 2) was 40 % for concentrations lower than or equal to 1 mg/kg, and 30 % for concentrations greater than 1 mg/kg.
开发并验证了一种分析方法,用于分析法国西印度群岛三种主要类型土壤(铁铝土、红壤和赤红壤)中的十氯酮,这些土壤中添加了用于修复过程的 Daramend®和堆肥改良剂,以及未添加的情况。该方法包括加压液体萃取后通过气相色谱-三重四极杆质谱联用进行分析。土壤中高含量的天然有机质以及测试用改良剂中额外的外源有机质导致提取物非常复杂。反式-非氯丹被用作萃取效率的校正物,添加 (13)C 十氯酮作为内标,以尽可能模拟十氯酮的行为并抑制其分析过程中的可能副作用。该方法的关键参数(线性、重复性、日间精密度、特异性、萃取效率和定量限)按照 NF T 90-210 标准方法进行了验证。定量限为 0.03 mg/kg。对于浓度低于或等于 1 mg/kg 的样品,不确定性(k = 2)为 40%,对于浓度大于 1 mg/kg 的样品,不确定性为 30%。