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Development of a method to profile 2- to 4-ring polycyclic aromatic hydrocarbons in saliva samples from smokers and non-smokers by headspace-solid-phase microextraction-gas chromatography-triple quadrupole tandem mass spectrometry.
Journal of Chromatography B ( IF 3 ) Pub Date : 2020-07-16 , DOI: 10.1016/j.jchromb.2020.122273
Patricia Martín Santos 1 , Laura Campo 2 , Luca Olgiati 2 , Elisa Polledri 3 , Miguel Del Nogal Sánchez 1 , Silvia Fustinoni 4
Affiliation  

This study reports the development of a method based on headspace (HS)-solid-phase microextraction (SPME)-gas chromatography (GC)-triple quadrupole tandem mass spectrometry (MS/MS) for the quantification of 2- to 4-ring polycyclic aromatic hydrocarbons (PAHs) in saliva samples. Eight unmetabolized compounds (naphthalene, acenaphthylene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene and pyrene) were quantified using six deuterated PAHs as surrogate internal standards. The absence of matrix effect allowed saliva samples to be quantified by external calibration method. The optimized method resulted easy, with minimal sample pre-treatment (homogenization of the sample), and it achieved the highest sensitivity up to date: limits of quantification (LOQ) were in the 0.8–26.4 ng L-1 range, with a significant improvement in comparison with the few existing methods. Intra- and inter-run precisions provided CV values <18.1%, and accuracies within 20% of the spiked concentration. The application of the method to the analysis of fresh saliva samples collected by spitting from smokers (n = 10) and non-smokers (n = 10) showed that PAHs were quantifiable in all samples and that smokers had higher levels of all compounds than non-smokers. These results show that the method is suitable for quantifying low-boiling PAHs in saliva samples from individuals exposed at different PAH levels.



中文翻译:

开发了一种通过顶空-固相微萃取-气相色谱-三重串联四极杆串联质谱法分析吸烟者和非吸烟者唾液样品中2至4环多环芳烃的方法。

这项研究报告了一种基于顶空(HS)-固相微萃取(SPME)-气相色谱(GC)-三重四极杆串联质谱(MS / MS)的方法的开发,该方法用于定量2至4环多环唾液样品中的芳烃(PAH)。使用六个氘代多环芳烃作为替代内标对八种未代谢的化合物(萘,、,、芴,菲,蒽,荧蒽和pyr)进行了定量。基质效应的不存在使唾液样品可以通过外部校准方法进行定量。经过优化的方法简便易行,只需进行最少的样品前处理(样品均质),并实现了迄今为止的最高灵敏度:定量限(LOQ)在0.8–26.4 ng L -1范围,与现有的几种方法相比有显着改善。批内和批间精度提供CV值<18.1%,且准确度在加标浓度的20%以内。该方法在分析从吸烟者(n  = 10)和非吸烟者(n  = 10)随地吐痰收集的新鲜唾液样品中的应用表明,在所有样品中PAHs均可量化,并且吸烟者的所有化合物含量均高于未吸烟者-吸烟者。这些结果表明,该方法适用于定量来自暴露于不同PAH水平的个体的唾液样品中的低沸点PAH。

更新日期:2020-07-25
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