Chromaleont s.r.l., c/o Department of Chemical, Biological, Pharmaceutical and Environmental Sciences, former Veterinary School, University of Messina, Viale G. Palatucci snc, Messina 98168, Italy.
Department of Mathematical and Computer Science, Physical Sciences and Earth Sciences, University of Messina, Viale F. Stagno d'Alcontres 31, Messina 98166, Italy.
J Chromatogr A. 2024 Sep 13;1732:465248. doi: 10.1016/j.chroma.2024.465248. Epub 2024 Aug 8.
The present study is based on the development of a straightforward method for the determination (semi-quantification) of 16 polycyclic aromatic hydrocarbons (PAHs) in extra virgin olive oil (EVOO) using "cryogenic-zone-compression" (CZC) gas chromatography-single quadrupole mass spectrometry (GC-QMS). The use of CZC (through a loop-type cryogenic modulator) to achieve enhanced signal-to-noise ratios (s/n), enabled a simplification of the sample preparation step. In fact, a single extraction process (using only 500 µL of acetonitrile) was performed prior to injection. The CZC GC-QMS method aligns with the principles of green analytical chemistry, and enabled an average s/n increase of 14-fold compared to conventional GC-QMS. The method limits of quantification were in the 0.07-8.33 µg kg range. Accuracy (at the 2 μg kg and 10 μg kg concentration levels) was in the 82-103 % range. Intra-day and inter-day precision (at 2 μg kg and 10 μg kg concentration levels) were in the 1.9-14.7 % and 5.9-9.1 % ranges, respectively, while the recovery values (at 10 µg kg) ranged from 24 % to 99 %. For all the PAHs investigated, a positive matrix effect was observed. Two PAHs were detected (in the selected-ion-monitoring mode) in six EVOOs among the ten samples (not more than one PAH per sample).
本研究基于开发一种直接的方法，用于使用“低温区压缩”（CZC）气相色谱-单四极杆质谱（GC-QMS）测定（半定量）特级初榨橄榄油（EVOO）中的 16 种多环芳烃（PAHs）。CZC（通过环型低温调制器）的使用实现了信号与噪声比（s/n）的增强，简化了样品制备步骤。事实上，在进样之前仅进行了一次提取过程（仅使用 500 µL 乙腈）。CZC GC-QMS 方法符合绿色分析化学的原则，与常规 GC-QMS 相比，平均 s/n 提高了 14 倍。方法的定量限在 0.07-8.33 µg kg 范围内。准确度（在 2 µg kg 和 10 µg kg 浓度水平）在 82-103%范围内。日内和日间精密度（在 2 µg kg 和 10 µg kg 浓度水平）分别为 1.9-14.7%和 5.9-9.1%，而回收率（在 10 µg kg）范围为 24%-99%。对于所有研究的 PAHs，均观察到正基质效应。在十个样品中的六个 EVOO 中（每个样品不超过一种 PAH），以选择离子监测模式检测到两种 PAHs。
