利用支撑液萃取和气相色谱-串联质谱法对血清多溴联苯醚进行人体生物监测。

IF 2.8 3区 工程技术 Q2 CHEMISTRY, ANALYTICAL Journal of separation science Pub Date : 2024-11-04 DOI:10.1002/jssc.70010
Miao Liu, Xiangyu Jia, Rongfei Peng, Zhijun Bai, Jun Yuan, Lei Tan
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引用次数: 0

摘要

本研究旨在利用气相色谱-串联质谱法开发并验证一种可靠的分析方法,用于定量检测人体血清中的多溴联苯醚(PBDEs)。我们比较了用于测定血清多溴联苯醚的液液萃取和支撑液萃取的程序空白、回收率和操作便利性。我们评估了不同萃取溶剂对多溴联苯醚回收率的影响。由于操作方便,我们选择了支撑液萃取法进行方法验证。该方法的线性、灵敏度和重现性令人满意,大多数多溴联苯醚同系物的检测范围为 0.10-5.00 微克/升,PBDE-154 和 PBDE-183 的检测范围为 0.20-10.0 微克/升,检测限为 2-48 纳克/升,基质效应为 94%-113% 。质量控制评估表明,回收率为 85% 至 110%,相对标准偏差小于 11%。所提议的方法被应用于 111 名健康成年人的生物监测,结果显示 90% 以上的样本中都能检测到多溴联苯醚。其中以 BDE-47 和 BDE-183 最为普遍,平均浓度分别为 4.13 纳克/升和 22.1 纳克/升。检测频率从 BDE-17 和 BDE-85 的 0.90% 到 BDE-47 的 25.2% 不等。男性的 BDE-183 平均浓度高于女性。
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Human Biomonitoring of Serum Polybrominated Diphenyl Ethers by Supported Liquid Extraction and Gas Chromatography Coupled With Tandem Mass Spectrometry

This study aims to develop and validate a robust analytical method for the quantification of polybrominated diphenyl ethers (PBDEs) in human serum using gas chromatography–tandem mass spectrometry. We compared procedural blanks, recoveries, and operational convenience of liquid–liquid extraction and supported liquid extraction for the determination of serum PBDEs. We evaluated different extraction solvents for their effect on PBDE recoveries. Supported liquid extraction was selected for method validation due to its operational convenience. The method demonstrated satisfactory linearity, sensitivity, and reproducibility, with the range of 0.10–5.00 µg/L for most PBDE congeners and 0.20–10.0 µg/L for PBDE-154 and PBDE-183, with limits of detection ranging from 2 to 48 ng/L, and with matrix effects ranging from 94% to 113%. Quality control assessments indicated that recoveries ranged from 85% to 110% and relative standard deviations of less than 11%. The proposed method was applied to biomonitoring of 111 healthy adults, revealing detectable levels of PBDEs in over 90% of the samples. BDE-47 and BDE-183 were the most prevalent, with mean concentrations of 4.13 and 22.1 ng/L, respectively. Detection frequencies ranged from 0.90% for BDE-17 and BDE-85 to 25.2% for BDE-47. Males had higher mean concentrations of BDE-183 than females.

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来源期刊
Journal of separation science
Journal of separation science 化学-分析化学
CiteScore
6.30
自引率
16.10%
发文量
408
审稿时长
1.8 months
期刊介绍: The Journal of Separation Science (JSS) is the most comprehensive source in separation science, since it covers all areas of chromatographic and electrophoretic separation methods in theory and practice, both in the analytical and in the preparative mode, solid phase extraction, sample preparation, and related techniques. Manuscripts on methodological or instrumental developments, including detection aspects, in particular mass spectrometry, as well as on innovative applications will also be published. Manuscripts on hyphenation, automation, and miniaturization are particularly welcome. Pre- and post-separation facets of a total analysis may be covered as well as the underlying logic of the development or application of a method.
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