Determination of polybrominated diphenyl ethers and polychlorinated biphenyls in human adipose tissue by large-volume injection - Narrow-bore capillary gas chromatography/electron impact low-resolution mass spectrometry
Determination of polybrominated diphenyl ethers and polychlorinated biphenyls in human adipose tissue by large-volume injection - Narrow-bore capillary gas chromatography/electron impact low-resolution mass spectrometry
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DOI：
10.1021/ac010784e
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发表时间：
2002-02-15
影响因子：
7.4
通讯作者：
Schepens, P
中科院分区：
文献类型：
--
作者：
Covaci, A;de Boer, J;Schepens, P
建立了一种测定人体脂肪组织中多溴联苯醚(PBDEs)的新方法。经过索氏提取和使用两个连续的含有酸性二氧化硅和酸性二氧化硅的固相萃取柱：中性二氧化硅：失活的碱性氧化铝(自上而下)的清理程序后，可以通过窄孔(0.10 mm I.D.)实现检测。采用大体积进样技术的毛细管气相色谱/电子轰击低分辨质谱仪。使用窄口径毛细管，可以在短时间(长达10分钟)内分析复杂混合物，节省50%或更多的传统色谱柱的分析时间，同时保持类似的分辨率。该方法允许在低于1 ng/g脂肪重量的浓度下测定五种主要的多溴联苯醚同系物(BDE28、47、99、100和153)。根据溴化程度的不同，所选离子模式的检出限在0.05至0.30 ng/g脂类重量之间变化。该方法的灵敏度可以与电子俘获电离的低分辨质谱学相媲美，同时获得了更好的选择性。在20个比利时人脂肪组织样本中，多溴二苯醚的水平在2.18至11.70纳克/克脂肪重量之间，与之前欧洲报告的数值相似。
A new analytical method has been developed for the quantification of polybrominated diphenyl ethers (PBDEs) in human adipose tissue samples. After Soxhlet extraction and a cleanup procedure using two successive solid-phase extraction cartridges containing acid silica and acid silica: neutral silica:deactivated basic alumina (from top to bottom), detection can been achieved by narrow-bore (0.10-mm i.d.) capillary gas chromatography/electron impact low-resolution mass spectrometry using a large-volume injection technique. Using narrow-bore capillaries, it is possible to analyze complex mixtures in a short time (up to 10 min), saving 50% or more of the analysis time of conventional columns while maintaining a similar resolution power. The method allows the determination of five major PBDE congeners (BDE 28, 47, 99, 100, and 153) at concentrations below 1 ng/g lipid weight. Detection limits in the selected ion mode varied between 0.05 and 0.30 ng/g lipid weights depending on the degree of bromination. The sensitivity of this method can compete with low-resolution mass spectrometry with electron capture ionization, while a much better selectivity is obtained. Levels of PBDEs in 20 Belgian human adipose tissue samples ranged between 2.18 and 11.70 ng/g lipid weight and were similar to previously reported values from Europe.