Comprehensive two-dimensional gas chromatography with isotope dilution time-of-flight mass spectrometry for the measurement of dioxins and polychlorinated biphenyls in foodstuffs - Comparison with other methods
Comprehensive two-dimensional gas chromatography with isotope dilution time-of-flight mass spectrometry for the measurement of dioxins and polychlorinated biphenyls in foodstuffs - Comparison with other methods
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DOI：
10.1016/j.chroma.2005.05.090
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发表时间：
2005-09-09
影响因子：
4.1
通讯作者：
De Pauw, E
中科院分区：
文献类型：
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作者：
Focant, JF;Eppe, G;De Pauw, E
建立了一套完整的二维气相色谱飞行时间质谱仪(GC-TOF-MS)实验装置，对食品样品中7种2，3，7，8-取代多氯二苯并-对二恶英(PCDDs)、10种2，3，7，8-取代多氯二苯并呋喃(PCDF)、4种非邻位多氯联苯(PCbs)、8种单邻位PCbs和6种指示剂多氯联苯(Aroclor 1260)进行了检测。使用40m RTX-500(0.18 mm I.D.，0.10µm DF)作为第一维度(D-1)，使用1.5nn BPX-50(0.10 mm I.D.，0.10µm DF)作为第二维度(2D)。GC-X-GC层析分离在45min内完成。使用C-13标记的同位素稀释法进行定量。在峰指定和定量之前，将所选定量离子的同位素比率与理论值进行核对。动态工作范围跨越三个数量级。2，3，7，8-TCDD的最低检出量为0.2pg。鱼、猪肉和牛奶样本也被考虑在内。在同类基础上，将GC x GC-ID-TOF-MS方法与参考GC-ID高分辨率质谱法(HRMS)和替代GC-ID串联时间四极杆离子存储质谱法(QIST-MS/MS)进行比较。每克样品的多氯联苯水平从低皮克(Pg)到低纳克(Ng)不等，不同方法之间的数据比较很好。就所有基质而言，按新鲜重量计算，PCDD/F处于较低的PG水平(0.05-3 PG)。GC-ID-TOF-MS和GC-QIST-MS/MS的相对标准偏差远高于GC-ID-HRMS，尤其是对低水平的猪肉和牛奶。在毒性当量(TEQ)的基础上，所有方法，包括二恶英响应的化学激活荧光素酶基因表达(DR-CALUX)分析，都产生了类似的反应。文中还给出了成本比较。(C)2005 Elsevier B.V.保留所有权利。
A comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GC x GC-TOF-MS) experimental setup was tested for the measurement of seven 2,3,7,8-substituted polychlorinated dibenzo-p-dioxins (PCDDs), ten 2,3,7,8-substituted polychlorinated dibenzofurans (PCDFs), four non-ortho-polychlorinated biphenyls (PCBs), eight mono-ortho-PCBs, and six indicator PCBs (Aroclor 1260) in foodstuff samples. A 40 m RTX-500 (0.18 mm I.D., 0.10 mu m df) was used as the first dimension (D-1) and a 1.5 nn BPX-50 (0.10 mm I.D., 0.10 mu m df) as the second dimension (2 D). The GC x GC chromatographic separation was completed in 45 min. Quantification was performed using C-13-label isotope dilution (11)). Isotope ratios of the selected quantification ions were checked against theoretical values prior to peak assignment and quantification. The dynamic working range spanned three orders of magnitude. The lowest detectable amount of 2,3,7,8-TCDD was 0.2 pg. Fish, pork, and milk samples were considered. On a congener basis, the GC x GC-ID-TOF-MS method was compared to the reference GC-ID high resolution mass spectrometry (HRMS) method and to the alternative GC-ID tandem-in-time quadrupole ion storage mass spectrometry (QIST-MS/MS). PCB levels ranged from low picogram (pg) to low nanogram (ng) per gram of sample and data compared very well between the different methods. For all matrices, PCDD/Fs were at a low pg level (0.05-3 pg) on a fresh weight basis. Although congener profiles were accurately described, RSDs of GC x GC-ID-TOF-MS and GC-QIST-MS/MS were much higher than for GC-ID-HRMS, especially for low level pork and milk. On a toxic equivalent (TEQ) basis, all methods, including the dioxin-responsive chemically activated luciferase gene expression (DR-CALUX) assay, produced similar responses. A cost comparison is also presented. (c) 2005 Elsevier B.V. All rights reserved.