This work describes a novel application of atmospheric pressure gas chromatography time-of-flight mass spectrometry (APGC-TOF-MS) combined with solid-phase microextraction (SPME) for the simultaneous analysis of hydrocarbons and naphthenic acids (NAs) species in raw and ozone-treated oil sands process water (OSPW). SPME method using polydimethylsiloxane (PDMS)-coated fibers was validated using gas chromatography with flame ionization detector (GC-FID) to ensure the SPME extractions were operated appropriately. The ionization pathways of the hydrocarbon species in OSPW in the APGC source were verified by analyzing a mixture of eight polyaromatic hydrocarbons which were ionized primarily via charge transfer to produce [M⁺] while NAs in OSPW were found to be ionized through protonation to generate [MH⁺] in the wet APGC source. SPME/APGC-TOF-MS analysis demonstrated a different composition profile in OSPW #1, with 74.5% of hydrocarbon species, 23.4% of O₂–NAs, and 2.1% of the oxidized NA species at extraction pH 2.0 compared with that obtained by UPLC-TOF-MS analysis (36.9% of O₂–NAs, 26.8% of O₃–NAs, 24.9% of O₄–NAs, 9.1% of O₅–NAs, 2.3% of O₆–NAs). Moreover, the peak areas of the total NAs and the total peak areas of NAs + hydrocarbons measured by SPME/APGC-TOF-MS correlated excellently with the total NA concentration determined by UPLC-TOF-MS (R² = 0.90) and the concentrations of the total acid-extractable organics determined by SPME/GC-FID (R² = 0.98), respectively. APGC-TOF-MS integrated with the SPME techniques could extend the range of target compounds and be a promising alternative to evaluate and characterize NAs and hydrocarbon in different water types.

这项工作描述了常压气相色谱飞行时间质谱（APGC-TOF-MS）结合固相微萃取（SPME）的新应用，用于同时分析原料和原料中的碳氢化合物和环烷酸（NAs）种类。臭氧处理的油砂工艺水（OSPW）。使用气相色谱和火焰离子化检测器（GC-FID）对使用聚二甲基硅氧烷（PDMS）涂层纤维的SPME方法进行了验证，以确保SPME提取操作正确。通过分析八种主要通过电荷转移被电离以产生[M ⁺ ]的聚芳烃的混合物，验证了APGC源中OSPW中碳氢化合物的电离途径，发现OSPW中的NAs通过质子化被电离以生成[M ⁺ ]。 MH湿APGC源中的⁺ ]。SPME / APGC-TOF-MS分析表明，在OSPW＃1中，与萃取法相比，在萃取pH 2.0下具有74.5％的碳氢化合物，23.4％的O ₂ -NAs和2.1％的氧化NA物种不同。 UPLC-TOF-MS分析（的O- 36.9％₂ -NAs，的O- 26.8％₃ -NAs，的O- 24.9％₄ -NAs，的O- 9.1％₅ -NAs，O- 2.3％₆ -NAs）。此外，SPME / APGC-TOF-MS测定的总NA的峰面积和NAs +烃的总峰面积与UPLC-TOF-MS测定的总NA浓度高度相关（R ²= 0.90）和通过SPME / GC-FID测定的可酸萃取的有机物总量（R ² = 0.98）。与SPME技术集成的APGC-TOF-MS可以扩展目标化合物的范围，是评估和表征不同水类型中NA和碳氢化合物的有前途的替代方法。