HIGH-RESOLUTION GAS-CHROMATOGRAPHIC HIGH-RESOLUTION MASS-SPECTROMETRIC ANALYSIS OF HUMAN-SERUM ON A WHOLE-WEIGHT AND LIPID BASIS FOR 2,3,7,8-TETRACHLORODIBENZO-P-DIOXIN
HIGH-RESOLUTION GAS-CHROMATOGRAPHIC HIGH-RESOLUTION MASS-SPECTROMETRIC ANALYSIS OF HUMAN-SERUM ON A WHOLE-WEIGHT AND LIPID BASIS FOR 2,3,7,8-TETRACHLORODIBENZO-P-DIOXIN
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DOI：
10.1021/ac00142a023
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发表时间：
1987-08-01
影响因子：
7.4
通讯作者：
NEEDHAM, LL
中科院分区：
文献类型：
--
作者：
PATTERSON, DG;HAMPTON, L;NEEDHAM, LL
我们描述了一种测量人血清中 2,3,7,8-四氯二苯并-对二恶英 (TCDD) 和其他 TCDD 异构体的分析方法；该方法采用高度特异性的净化程序和高分辨率气相色谱/高分辨率质谱分析。以[13C12]-2,3,7,8-TCDD为内标，通过同位素稀释技术对2,3,7,8-TCDD进行定量。其他 TCDD 异构体是通过使用已发布的相对响应因子来估计的。 200 克样品的 1.25 千万分之一 (ppq) 检测限足以测定人血清样本中的 2,3,7,8-TCDD 浓度。该方法经过修改，可用于分析 50 g 和 10 g 血清样品。分析加标样品的结果证明了分析的准确性。该方法被证明不受许多潜在干扰化合物的影响。使用一系列质量控制材料来验证系统性能。对于含有 25.8 ppq 天然 2,3,7,8-TCDD 的 200 g 样品，观察到变异系数 (CV) 为 13.0% (n = 20)。对于来自强化了 2,3,7,8-TCDD（万亿分之 1.9，n = 22）的池中的 10 克样品，观察到 CV 为 15.5%。
We describe an analytical method to measure 2,3,7,8-tetrachlorodibenzo-p-dioxin (TCDD) and other TCDD isomers in human serum; the method uses a highly specific cleanup procedure and high-resolution gas chromatography/high-resolution mass spectrometry. The 2,3,7,8-TCDD is quantified by the isotope dilution technique with [13C12]-2,3,7,8-TCDD as the internal standard. Other TCDD isomers are estimated by using published relative response factors. The 1.25 part-per-quadrillion (ppq) limit of detection for 200-g samples is more than adequate for determining 2,3,7,8-TCDD concentrations in human serum specimens. The method is modified for analyzing 50-g and 10-g serum samples. Analytical accuracy is demonstrated by the results obtained in analyzing spiked samples. The method is shown to be unaffected by a number of potentially interfering compounds. A series of quality control material is used to verify system performance. For 200-g samples containing 25.8 ppq of native 2,3,7,8-TCDD, a coefficient of variation (CV) of 13.0% is observed (n = 20). For 10-g samples from a pool fortified with 2,3,7,8-TCDD (1.9 parts per trillion, n = 22), a CV of 15.5% is observed.