Lara-Gonzalo Azucena, Sánchez-Uría José Enrique, Segovia-García Eva, Sanz-Medel Alfredo
Department of Physical and Analytical Chemistry, University of Oviedo, C/ Julian Clavería 8, 33006 Oviedo, Spain.
Talanta. 2008 Feb 15;74(5):1455-62. doi: 10.1016/j.talanta.2007.09.036. Epub 2007 Oct 2.
The use of two automated sample preparation techniques, solid-phase microextraction (SPME) and purge and trap (P&T) systems are critically compared for the GC-MS determination of eight volatile organic compounds (VOCs), including trihalomethanes (THMs), in drinking water samples. Compounds chosen for the comparison are regulated by Spanish and European official guidelines for drinking waters. Experimental parameters investigated for the two sample preparation techniques included SPME type of fibers, SPME modality, P&T gas flow, extraction and desorption times and desorption temperatures. Thus, optimal experimental conditions have been worked out for the SPME and P&T techniques. Under such optimised conditions, detection limits, precision and accuracy were evaluated. Both methods fulfilled the values that the official guidelines establish. The P&T-GC-MS method offers LDs ranged from 0.004 to 0.2 ng mL(-1), repeatabilities below 6% and recoveries between 81 and 117%; while LDs ranging from 0.008 to 0.7 ng mL(-1), 1-12% R.S.D. and recoveries from 80 to 119% were achieved with the SPME-GC-MS method. Finally, we chose P&T-GC-MS method as the best for this determination and we validate this methodology by its application to the analysis of an Aquacheck Interlaboratory Exercise.
本文对两种自动样品制备技术——固相微萃取(SPME)和吹扫捕集(P&T)系统进行了严格比较,用于气相色谱-质谱联用(GC-MS)测定饮用水样品中的8种挥发性有机化合物(VOCs),包括三卤甲烷(THMs)。用于比较的化合物受西班牙和欧洲饮用水官方指南的监管。针对这两种样品制备技术研究的实验参数包括SPME纤维类型、SPME模式、P&T气体流量、萃取和解吸时间以及解吸温度。因此,已确定了SPME和P&T技术的最佳实验条件。在这种优化条件下,评估了检测限、精密度和准确度。两种方法均符合官方指南规定的值。P&T-GC-MS方法的检测限范围为0.004至0.2 ng mL(-1),重复性低于6%,回收率在81%至117%之间;而SPME-GC-MS方法的检测限范围为0.008至0.7 ng mL(-1),相对标准偏差(R.S.D.)为1-12%,回收率为80%至119%。最后,我们选择P&T-GC-MS方法作为此测定的最佳方法,并通过将其应用于Aquacheck实验室间比对实验的分析来验证该方法。