食用油中矿物油饱和烃和矿物油芳烃的离线固相萃取与分离以及采用火焰离子化检测器的气相色谱分析
Offline Solid-Phase Extraction and Separation of Mineral Oil Saturated Hydrocarbons and Mineral Oil Aromatic Hydrocarbons in Edible Oils, and Analysis via GC with a Flame Ionization Detector.
作者信息
Ruiz José Luis Hidalgo, Liébanas Javier Arrebola, Vidal José Luis Martínez, Garrido Frenich Antonia, González Roberto Romero
机构信息
Center for Research in Mediterranean Intensive Agrosystems and Agri-Food Biotechnology (CIAIMBITAL), Department of Chemistry and Physics, Analytical Chemistry Area, Agrifood Campus of International Excellence ceiA3, University of Almería, Carretera de Sacramento s/n, E-04120 Almería, Spain.
出版信息
Foods. 2021 Aug 28;10(9):2026. doi: 10.3390/foods10092026.
A method was developed for the determination of mineral oil saturated hydrocarbons (MOSH) and mineral oil aromatic hydrocarbons (MOAH) in edible oils, achieving similar limits of quantification than those obtained by online extraction methodologies, i.e., 0.5 mg/kg. The isolation of MOSH and MOAH was performed in a silver nitrated silica gel stationary phase prior to their analysis by gas chromatography-flame ionization detector (GC-FID). To improve the sensitivity, the simulated on-column injection method, using a suitable liner, was optimized. The method was validated at 0.5, 10.0 and 17.9 mg/kg, and recoveries ranged from 80 to 110%. Intra and inter-day precision were evaluated at the same levels, and relative standard deviation (RSD) was lower than 20%. The method was applied to a total of 27 samples of different types of oil previously analyzed in an accredited laboratory, detecting MOSH up to 79.2 mg/kg and MOAH up to 22.4 mg/kg.
开发了一种测定食用油中矿物油饱和烃（MOSH）和矿物油芳烃（MOAH）的方法，其定量限与在线萃取方法获得的定量限相似，即0.5 mg/kg。在通过气相色谱 - 火焰离子化检测器（GC-FID）分析之前，在硝酸银硅胶固定相中进行MOSH和MOAH的分离。为提高灵敏度，使用合适的衬管对模拟柱上进样方法进行了优化。该方法在0.5、10.0和17.9 mg/kg水平进行了验证，回收率在80%至110%之间。在相同水平下评估了日内和日间精密度，相对标准偏差（RSD）低于20%。该方法应用于之前在认可实验室分析过的总共27个不同类型油样，检测到MOSH高达79.2 mg/kg，MOAH高达22.4 mg/kg。
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