Zhao Jiaying, Li Xiaomin, Lu Xiaohua, Zhang Qinghe, Zhang Weibing
College of Chemistry and Chemical Engineering, Qiqihar University, Qiqihar 161006, China.
Division of Chemical Metrology and Analytical Science, National Institute of Metrology, Beijing 100029, China.
Se Pu. 2017 Jul 8;35(7):748-754. doi: 10.3724/SP.J.1123.2017.03040.
A method for the determination of four polycyclic aromatic hydrocarbons (PAHs) such as benzo[]anthracene, chrysene, benzo[]fluoranthene and benzo[]pyrene in olive oil by high performance liquid chromatography-fluorescent detection (HPLC-FLD) was developed. The olive oil samples were diluted with isopropanol and cleaned-up by a solid phase extraction cartridge with specificity. Critical isomers were separated by gradient elution with water-acetonitrile on an Agilent ZORBAX Eclipse PAH column (100 mm×2.1 mm, 1.8 μ m). The calibration was performed by the use of matrix-matched calibration standards. The results showed that there were good linear relationships for the four PAHs in the range of 2.4-40 μ g/L with correlation coefficients of 0.9990-0.9999. The limits of quantification (LOQs) ranged from 0.147 to 0.413 μ g/L, and the recoveries of the spiked samples ranged from 95.5% to 103.2%. The intra-day and inter-day precisions were in the ranges of 0.10%-1.69% and 2.48%-2.93% (=5), respectively. The method has the characteristics of high sensitivity, low detection limit and good precision, and is suitable for rapid and accurate quantitative detection of the four PAHs in olive oil.
建立了一种采用高效液相色谱 - 荧光检测法（HPLC - FLD）测定橄榄油中苯并[a]蒽、 Chrysene、苯并[b]荧蒽和苯并[a]芘这四种多环芳烃（PAHs）的方法。橄榄油样品用异丙醇稀释，并通过具有特异性的固相萃取柱进行净化。关键异构体在安捷伦ZORBAX Eclipse PAH柱（100 mm×2.1 mm，1.8μm）上采用水 - 乙腈梯度洗脱进行分离。采用基质匹配校准标准品进行校准。结果表明，四种PAHs在2.4 - 40μg/L范围内具有良好的线性关系，相关系数为0.9990 - 0.9999。定量限（LOQs）范围为0.147至0.413μg/L，加标样品的回收率范围为95.5%至103.2%。日内和日间精密度分别在0.10% - 1.69%和2.48% - 2.93%（n = 5）范围内。该方法具有灵敏度高、检测限低和精密度好的特点，适用于橄榄油中四种PAHs的快速准确定量检测。
