Malavia J, Santos F J, Galceran M T
Analytical Chemistry Department, University of Barcelona, Martí i Franqués 1-11, 08028 Barcelona, Spain.
J Chromatogr A. 2008 Apr 4;1186(1-2):302-11. doi: 10.1016/j.chroma.2007.11.089. Epub 2007 Dec 4.
Two gas chromatography-mass spectrometry systems equipped with an ion-trap mass analyzer working in tandem mode (GC-MS-MS) were evaluated for the determination of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs) and dioxin-like polychlorinated biphenyls (PCBs) in food samples. The performance of the two ion-trap instruments, which dispose of an external ion source (ThermoFinnigan GCQ/Polaris) and internal ionization (Varian Saturn 2,200), have been compared in terms of linearity, repeatability, limit of detection and long-term precision. Both instruments provided similar run-to-run and day-to-day precisions, ranging from 2% to 8% and between 2% and 13%, and instrumental limits of detection between 0.09 and 0.36 pg injected for PCDD/Fs and from 0.03 to 0.09 pg injected for dioxin-like PCBs. Although both instruments seem to be suitable for food analysis, only the use of external ionization allowed to achieve reliable results for PCDD/F determination at concentrations close to the maximum residue levels established by the EU for foods. Internal ionization provides high limits of detection (from 10- to 30-fold higher) and worse precision (RSD, 14-43%). In contrast, for dioxin-like PCBs both instruments allowed to obtain excellent results with precisions lower than 15%.
评估了两台配备串联模式工作的离子阱质量分析仪的气相色谱 - 质谱联用系统(GC - MS - MS),用于测定食品样品中的多氯代二苯并 - p - 二恶英和二苯并呋喃(PCDD/Fs)以及类二恶英多氯联苯(PCBs)。比较了这两台离子阱仪器的性能,它们分别配置外部离子源(ThermoFinnigan GCQ/Polaris)和内部电离源(Varian Saturn 2,200),比较内容包括线性、重复性、检测限和长期精密度。两台仪器的批内和批间精密度相似,PCDD/Fs的批内精密度为2%至8%,批间精密度为2%至13%,检测限为每进样0.09至0.36 pg;类二恶英PCBs的批内精密度为2%至8%,批间精密度为2%至13%,检测限为每进样0.03至0.09 pg。尽管两台仪器似乎都适用于食品分析,但只有使用外部电离才能在接近欧盟规定的食品最大残留限量的浓度下可靠地测定PCDD/Fs。内部电离的检测限很高(高出10至30倍)且精密度较差(相对标准偏差,RSD为14 - 43%)。相比之下,对于类二恶英PCBs,两台仪器都能获得优异的结果,精密度低于15%。