Laboratories Cavendish S.L.U.™ Research Department, E-18220 Granada, Spain.
Talanta. 2012 Jan 30;89:322-34. doi: 10.1016/j.talanta.2011.12.037. Epub 2011 Dec 19.
A multi-residue method for the analysis of semi-volatile organic pollutants in inland groundwater (river water) at ultra-trace levels in compliance with the European Water Framework Directive (WFD) has been developed and validated by stir bar sorptive extraction (SBSE) and thermal desorption coupled with gas chromatography-triple quadrupole mass spectrometry (SBSE-TD-GC-MS/MS(QqQ)). The method includes various families of compounds included in the WFD and other compounds listed as persistent organic pollutants that are banned in the Stockholm Convention of Persistent Organic Pollutants, such as polychlorinated biphenyls, polycyclic aromatics hydrocarbons, and other pesticides not included in the WFD. The method also can be applied for compliance with regional environmental laws. Extraction conditions were optimised in order to analyse simultaneously analytes with very different polarities and octanol-water partition coefficients, which is an important parameter in the optimisation of a SBSE method. The quantification limits (LOQs) obtained ranged from 0.14 to 10 ng L(-1), lower that others presented in previous publications, and complies with the requirement for analytical methods to be used in the analysis of the compounds included in the WFD. Several quality parameters as linearity, trueness and precision were studied with good results, and also uncertainty was estimated. The WFD requires that the level of uncertainty must be lower than 50%, and this requirement was met for all compounds. Precision (in terms of RSD) was lower than 30%, recoveries ranged between 74 and 111%, and determination coefficients were higher than 0.990 for all analytes. Different factors that affect the SBSE procedure were optimised. GC-MS/MS parameters have also been revised. The accuracy of the method was tested participating in a proficiency testing scheme for each group of analytes.
已开发并验证了一种多残留方法，用于分析内陆地下水（河水）中的痕量水平的半挥发性有机污染物，符合欧洲水框架指令（WFD）的要求。该方法通过搅拌棒吸附萃取（SBSE）和热解吸与气相色谱-三重四极杆质谱联用（SBSE-TD-GC-MS/MS(QqQ)）实现。该方法包括 WFD 中包含的各种化合物家族，以及斯德哥尔摩持久性有机污染物公约中禁止的持久性有机污染物列为持久性有机污染物的其他化合物，如多氯联苯、多环芳烃和其他不在 WFD 中的农药。该方法也可用于遵守区域环境法规。为了同时分析具有非常不同极性和辛醇-水分配系数的分析物，优化了萃取条件，这是优化 SBSE 方法的一个重要参数。获得的定量限（LOQ）范围为 0.14 至 10ng/L-1，低于以前出版物中提出的其他 LOQ，符合用于分析 WFD 中包含的化合物的分析方法的要求。研究了几个质量参数，如线性、准确度和精密度，结果良好，还估计了不确定性。WFD 要求不确定性水平必须低于 50%，所有化合物都满足这一要求。精密度（以 RSD 表示）低于 30%，回收率在 74%至 111%之间，所有分析物的测定系数均高于 0.990。优化了影响 SBSE 过程的不同因素。还修订了 GC-MS/MS 参数。通过参加每个分析物组的能力验证计划，测试了该方法的准确性。
