灵敏仪器法定量测定人血清样品中高溴化阻燃剂。

IF 1.7 4区 农林科学 Q3 CHEMISTRY, ANALYTICAL
Cristina Grande, Argelia Castaño, Juan José Ramos
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引用次数: 0

摘要

背景:高溴化阻燃剂(BFRs)可从消费品(如电气和电子设备)释放到环境中,并通过不同途径进入人体。由于它们的毒性和法规,了解它们在人体样本中的水平和趋势是非常重要的。然而,一些这些化合物的色谱血清分析代表了目前在一般人群的挑战。目的:优化并验证一种基于气相色谱-质谱联用的仪器分析方法,该方法结合简单的样品制备程序,可以分析普通人群血清样品中的十溴二苯醚(BDE-209)、十溴二苯乙烷(DBDPE)和四溴双酚a -双(2,3-二溴丙基醚)(TBBPA-DBPE)。方法:为了最大限度地减少仪器分析过程中的高降解,对进样量、载体流速和柱长等GC参数进行了评估和优化。该仪器方法结合固相萃取(SPE)和多层硅胶柱纯化,仅使用1ml血清即可获得令人满意的分析结果。结果:在0.01、0.05、0.2 ng/mL三个加峰水平下,评价了完整方法的性能。回收率在87-108%之间,而日间测量的相对标准偏差一般低于19%。检出限为0.0045 ~ 0.0070 ng/mL。优化后的方法成功地应用于普通人群实际人体样品中所研究污染物的测定。结论:提出的方法有助于将这些环境污染物纳入人类生物监测(HBM)研究,增加对普通人群水平和趋势的了解。亮点:气相色谱-质谱参数优化,以尽量减少仪器分析降解。成功应用于普通人群的人血清样本。首次报道四溴双酚A双(2,3-二溴丙基醚)人血清水平。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
Sensitive Instrumental Method for Quantitative Determination of High-Brominated Flame Retardants in Human Serum Samples.

Background: High-brominated flame retardants (BFRs) can be released into the environment from consumer products, such as electric and electronic equipment, and enter the human body by different pathways. Because of their toxicity and the regulations, it is very relevant to know their levels and trends in human samples. However, chromatographic serum analysis of some of these compounds represents nowadays a challenge in the general population.

Objective: To optimize and validate an instrumental method based on gas chromatography coupled to mass spectrometry, which, together with a simple sample preparation procedure, allows the analysis of decabromodiphenyl ether (BDE-209), decabromodiphenyl ethane (DBDPE), and tetrabromobisphenol A-bis(2,3-dibromopropyl ether) (TBBPA-DBPE) in human serum samples from the general population.

Method: To minimize the high degradation during instrumental analysis, GC parameters such as injection volumes, carrier flow rates, and column lengths were assessed and optimized. This instrumental approach in combination with solid-phase extraction (SPE) followed by multilayer silica gel column purification allowed satisfactory analysis using only 1 mL of serum.

Results: The performance of the complete method was evaluated at three spiking levels, 0.01, 0.05, and 0.2 ng/mL. Recoveries in the range 87-108% were obtained whereas the relative standard deviation in interday measurements, were, in general, lower than 19%. Limits of detection were in the range of 0.0045-0.0070 ng/mL. The optimized procedure was successfully applied to the determination of the investigated pollutants in real human samples of general population.

Conclusions: The proposed method could contribute to the inclusion of these environmental pollutants in human biomonitoring (HBM) studies, increasing the knowledge of levels and trends in the general population.

Highlights: GC-MS parameters optimization to minimize instrumental analytes degradation. Successful application to human serum samples from the general population. Tetrabromobisphenol A bis(2,3-dibromopropyl ether) human serum levels are reported for the first time.

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来源期刊
Journal of AOAC International
Journal of AOAC International 医学-分析化学
CiteScore
3.10
自引率
12.50%
发文量
144
审稿时长
2.7 months
期刊介绍: The Journal of AOAC INTERNATIONAL publishes the latest in basic and applied research in analytical sciences related to foods, drugs, agriculture, the environment, and more. The Journal is the method researchers'' forum for exchanging information and keeping informed of new technology and techniques pertinent to regulatory agencies and regulated industries.
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