Department of Hydrogeology and Analytical Chemistry, University of Almería, 04120 Almería, Spain.
Anal Bioanal Chem. 2011 Feb;399(6):2043-59. doi: 10.1007/s00216-010-4236-0. Epub 2010 Oct 3.
This work compares two miniaturised sample preparation methods, solid phase microextraction (SPME) and hollow fiber liquid phase microextraction (HF-LPME), in combination with gas chromatography coupled to tandem mass spectrometry with a triple quadrupole analyzer for the determination of 77 pesticides in drinking water. In the case of SPME, extraction temperature and time were optimized by experimental design, although other parameters, as desorption time, pH, and ionic strength, were also evaluated. The extraction and desorption solvents [octanol/dihexyl ether (75:25, v/v) and cyclohexane, respectively], as well as the extraction and desorption time, ionic strength, and pH, were studied for the HF-LPME procedure. Under the optimal conditions, recoveries (70.2-113.5% for SPME and 70.0-119.5% for HF-LPME), intra-day precision (2.1-19.4% for SPME and 4.3-22.5% for HF-LPME), inter-day precision (5.2-21.5% for SPME and 8.4-27.3% for HF-LPME), and limits of detection, between 0.1 and 28.8 ng/L for SPME and 0.2 and 47.1 ng/L for HF-LPME and overall uncertainty (9.6-25.2% for SPME and 13.3-27.5% for HF-LPME) were established for both extraction procedures. Finally, the proposed methods were successfully applied to the analysis of 41 drinking water samples, and similar results were obtained with both extraction approaches.
本工作比较了两种微型化样品前处理方法，固相微萃取（SPME）和中空纤维液相微萃取（HF-LPME），结合气相色谱-串联质谱三重四极杆分析器，用于测定饮用水中的 77 种农药。在 SPME 情况下，通过实验设计优化了萃取温度和时间，尽管还评估了其他参数，如解吸时间、pH 值和离子强度。萃取和洗脱溶剂[辛醇/二乙醚（75:25，v/v）和环己烷]，以及萃取和洗脱时间、离子强度和 pH 值，也对 HF-LPME 程序进行了研究。在最佳条件下，回收率（SPME 为 70.2-113.5%，HF-LPME 为 70.0-119.5%）、日内精密度（SPME 为 2.1-19.4%，HF-LPME 为 4.3-22.5%）、日间精密度（SPME 为 5.2-21.5%，HF-LPME 为 8.4-27.3%）和检出限，SPME 为 0.1-28.8ng/L，HF-LPME 为 0.2-47.1ng/L，总不确定度（SPME 为 9.6-25.2%，HF-LPME 为 13.3-27.5%），这两种萃取方法均建立了这两种萃取方法。最后，将所提出的方法成功应用于 41 个饮用水样品的分析，两种萃取方法均得到了相似的结果。
