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Development and validation of a multi-pollutant method for the analysis of polycyclic aromatic hydrocarbons, synthetic musk compounds and plasticizers in atmospheric particulate matter (PM2.5)
Talanta Open ( IF 4.1 ) Pub Date : 2021-07-18 , DOI: 10.1016/j.talo.2021.100057
Joel Sánchez-Piñero 1 , Jorge Moreda-Piñeiro 1 , Carmen Moscoso-Pérez 1 , Verónica FernándezGonzález 1 , Darío Prada-Rodríguez 1 , Purificación López-Mahía 1
Affiliation  

Exposure to atmospheric particulate matter (PM) associated pollutants is a global concern due to the risk posed in human health after inhalation. In this study, a simple and sensitive multi-residue method is developed for the analysis of 50 organic pollutants, comprising 18 polycyclic aromatic hydrocarbons (PAHs), 12 phthalate esters (PAEs), 12 organophosphorus flame retardants (OPFRs), 6 synthetic musk compounds (SMCs) and 2 bisphenols in PM2.5 samples. The method consists of three cycles of ultrasonic assisted solvent extraction and vortex (UASE + vortex), followed by a vortex-assisted dispersive solid phase extraction (d-SPE) clean-up and a final determination step by using programmed temperature vaporization-gas chromatography-tandem mass spectrometry (PTV-GC-MS/MS). Experimental conditions concerning clean-up adsorbents (alumina, silica gel and Florisil®) and filters (glass fibre, PTFE and nylon), as well as PTV-GC-MS/MS conditions were studied. In addition, the use of SRM (selected reaction monitoring) mode in MS-MS, as well as matrix-matched calibration together with labelled subrogate standards, resulted in successfully validation results for most of the compounds due to the high sensitivity, minimization of matrix effects and recovering losses compensation. The proposed method was validated in terms of linearity, limits of detection and quantification (LODs and LOQs), analytical recoveries by analysing a spiked composite sample (PM2.5) at three spiking levels and intra-day and inter-day precision. Moreover, an urban particulate matter standard reference material (SRM 1648a) was analysed to assess PAHs determination accuracy. Furthermore, applicability of the method was proved by analysing 12 PM2.5 samples from an industrial area. Among all studied pollutants, bisphenol A (BPA) was the most predominant with an average concentration of 5000 pg m−3, followed by bis(2-ethylhexyl) phthalate (DEHP) and diisobutyl phthtalate (DiBP) with 1990 pg m−3 and 632 pg m-3, respectively. Concerning OPFRs, average concentrations between 345 – 253 pg m−3 were found for triphenyl phosphine oxide (TPPO), tris(chloropropyl) phosphate (TCPP), tri-iso-butyl phosphate (TiBP) and tris(2-butoxyethyl) phosphate (TBOEP). Finally, the highest PAHs levels were found for 5-6 ring-number PAHs (Σ5-6 rings PAHs) with an average concentration of 2680 pg m−3, while only 2 SMCs were quantitated accounting for 17.5 pg m−3 by average.



中文翻译:

用于分析大气颗粒物 (PM 2.5 )中多环芳烃、合成麝香化合物和增塑剂的多污染物方法的开发和验证

由于吸入后对人体健康构成风险,暴露于大气颗粒物 (PM) 相关污染物是一个全球性的问题。本研究开发了一种简单、灵敏的多残留方法,用于分析 50 种有机污染物,包括 18 种多环芳烃 (PAH)、12 种邻苯二甲酸酯 (PAE)、12 种有机磷阻燃剂 (OPFR)、6 种合成麝香化合物(SMC) 和 PM 2.5 中的2 个双酚样品。该方法包括三个超声波辅助溶剂萃取和涡旋 (UASE + 涡旋) 循环,然后是涡旋辅助分散固相萃取 (d-SPE) 净化和使用程序升温汽化-气相色谱法的最终测定步骤-串联质谱(PTV-GC-MS/MS)。研究了有关净化吸附剂(氧化铝、硅胶和 Florisil®)和过滤器(玻璃纤维、PTFE 和尼龙)的实验条件,以及 PTV-GC-MS/MS 条件。此外,在 MS-MS 中使用 SRM(选择反应监测)模式,以及基质匹配校准和标记的替代标准,由于高灵敏度、最小化基质,成功验证了大多数化合物的结果影响和恢复损失赔偿。2.5 ) 在三个尖峰水平和日内和日间精度。此外,还分析了城市颗粒物标准参考物质 (SRM 1648a) 以评估 PAH 测定的准确性。此外,通过分析来自工业区的12 个 PM 2.5样品证明了该方法的适用性。在所有研究的污染物中,双酚 A (BPA) 是最主要的,平均浓度为 5000 pg m -3,其次是邻苯二甲酸双(2-乙基己基)酯(DEHP)和邻苯二甲酸二异丁酯(DiBP),平均浓度为1990 pg m -3和分别为632 pg m -3。关于 OPFR,平均浓度在 345 – 253 pg m -3 之间发现三苯基氧化膦 (TPPO)、磷酸三(氯丙基)酯 (TCPP)、磷酸三异丁酯 (TiBP) 和磷酸三 (2-丁氧基乙基) 酯 (TBOEP)。最后,发现 5-6 环数多环芳烃(Σ 5-6 环多环芳烃)的PAH 水平最高,平均浓度为 2680 pg m -3,而只有 2 种 SMC 被定量,平均为 17.5 pg m -3 .

更新日期:2021-07-23
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