A Sensitive Online SPE-LC–APCI–MS/MS Method for Simultaneous Determination of 17 Nitrated and Oxygenated Polycyclic Aromatic Hydrocarbons in Atmospheric Particulate Matter

IF 1.2 4区化学 Q4 BIOCHEMICAL RESEARCH METHODS

Chromatographia Pub Date : 2023-10-05 DOI:10.1007/s10337-023-04280-1

Chao Wang, Weihong Zhu, Zongbo Shi, Jianjun Li

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Abstract

A highly sensitive method was developed for the determination of 17 nitrated and oxygenated polycyclic aromatic hydrocarbons (NPAHs and OPAHs) in PM_2.5 using an ultrasound-assisted extraction (UAE)-online solid phase extraction (online SPE)-liquid chromatography-tandem mass spectrometry (LC/MS). The method underwent comprehensive optimization, encompassing UAE solvents and times, extract filtering, online SPE condition and LC/MS condition. Isomeric separation and detection of mononitro-PAHs, dinitro-PAHs, and OPAHs were achieved based on the proposed MS/MS fragmentation pathway in negative mode atmospheric pressure chemical ionization. Taking the advantage of online SPE, the method achieved lower limits of detection (NPAHs: 0.001 ~ 0.042 μg L⁻¹, OPAHs: 0.01 ~ 0.038 μg L⁻¹). Recovery ranged from 64% ~ 108% at three spiking levels (0.25, 1.0 and 10.0 μg L⁻¹) with the relative standard deviations (RSDs) of 3% ~ 23%. This study represents first application of LC/MS methodology for the quantification of three carcinogenic dinitro-PAHs (1,3-dinitropyrene, 1,6-dinitropyrene, 1,8-dinitropyrene) in atmospheric PM_2.5. The established method was successfully employed to determine the wide range concentrations of various NPAHs and OPAHs (∑NPAH: 9.4 ~ 303.3 pg m⁻³, ∑OPAHs: 125.2 ~ 1948.1 pg m⁻³) in PM_2.5 samples collected in Beijing during the summer and winter seasons.

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灵敏在线SPE-LC–APCI–MS/MS法同时测定大气颗粒物中17种硝化和氧化多环芳烃

采用超声辅助萃取（UAE）-在线固相萃取（SPE）-液相色谱-串联质谱（LC/MS）测定PM2.5中17种硝化和氧化多环芳烃（NPAHs和OPAHs）。该方法进行了全面优化，包括UAE溶剂和时间、提取物过滤、在线SPE条件和LC/MS条件。基于所提出的负模式常压化学电离MS/MS裂解途径，实现了单硝基多环芳烃、二硝基多环芳烃和OPAHs的异构体分离和检测。利用在线SPE的优势，该方法实现了较低的检测极限（NPAHs:0.001 ~ 0.042μg L−1，OPAH:0.01 ~ 0.038μg L−1）。回收率为64% ~ 在三种加标水平（0.25、1.0和10.0μg L−1）下为108%，相对标准偏差（RSD）为3% ~ 23%。本研究首次应用LC/MS方法对大气PM2.5中的三种致癌二硝基多环芳烃（1,3-二硝基、1,6-二硝基和1,8-二硝基）进行定量。所建立的方法成功地用于测定各种NPAHs和OPAHs的宽范围浓度（∑NPAH:9.4 ~ 303.3 pg m−3，∑OPAH:125.2 ~ 1948.1 pg m−3）。

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来源期刊

Chromatographia 化学-分析化学

CiteScore

3.40

自引率

5.90%

发文量

103

审稿时长

2.2 months

期刊介绍： Separation sciences, in all their various forms such as chromatography, field-flow fractionation, and electrophoresis, provide some of the most powerful techniques in analytical chemistry and are applied within a number of important application areas, including archaeology, biotechnology, clinical, environmental, food, medical, petroleum, pharmaceutical, polymer and biopolymer research. Beyond serving analytical purposes, separation techniques are also used for preparative and process-scale applications. The scope and power of separation sciences is significantly extended by combination with spectroscopic detection methods (e.g., laser-based approaches, nuclear-magnetic resonance, Raman, chemiluminescence) and particularly, mass spectrometry, to create hyphenated techniques. In addition to exciting new developments in chromatography, such as ultra high-pressure systems, multidimensional separations, and high-temperature approaches, there have also been great advances in hybrid methods combining chromatography and electro-based separations, especially on the micro- and nanoscale. Integrated biological procedures (e.g., enzymatic, immunological, receptor-based assays) can also be part of the overall analytical process.