Bureau of Quality and Safety of Food, Department of Medical Science, Ministry of Public Health, Tivanond Road, Nonthaburi 11000, Thailand.
Food Chem. 2013 Dec 1;141(3):2720-6. doi: 10.1016/j.foodchem.2013.05.092. Epub 2013 May 25.
Low-temperature cleanup, which is a simple and cost-efficient sample preparation technique that allows the convenient treatment of multiple samples simultaneously, was developed in conjunction with solid-phase extraction (SPE) cleanup for the determination of 16 polycyclic aromatic hydrocarbons (PAHs) in refined and used edible oil samples by high-performance liquid chromatography with fluorescence detection (HPLC-FLD). Samples are extracted with a small amount of organic solvent and most of lipids in the extract were removed by low-temperature cleanup. SPE cartridge was used to further cleanup prior to HPLC-FLD analysis. Optimum extraction of low-temperature cleanup was achieved when using two extractions with a 4:1 (v/v) mixture of acetonitrile: acetone as the extraction solvent, freezing at between -18 °C and -25 °C for 24 h and then cleanup with an Alumina-N SPE cartridge. The PAH recoveries were 45.9-118.5%, with limit of detection (LOD) and limit of quantitation (LOQ) values of 0.13-3.13 μg/kg and 0.25-6.25 μg/kg across the 16 tested PAHs, respectively. The validated method was successfully applied for the determination of PAHs in reference materials of olive oil and real refined and used edible oil samples.
低温净化是一种简单且经济高效的样品制备技术，可同时方便地处理多个样品。该技术与固相萃取（SPE）净化相结合，用于通过高效液相色谱荧光检测（HPLC-FLD）测定精制和使用过的食用油样品中的 16 种多环芳烃（PAHs）。样品用少量有机溶剂提取，提取物中的大部分脂质通过低温净化去除。在进行 HPLC-FLD 分析之前，使用 SPE 柱进一步进行净化。当使用 4:1（v/v）的乙腈：丙酮混合物作为提取溶剂进行两次提取，在-18°C 至-25°C 下冷冻 24 小时，然后用氧化铝-N SPE 柱进行净化时，可实现低温净化的最佳提取效果。PAH 的回收率为 45.9-118.5%，在 16 种测试的 PAHs 中，检出限（LOD）和定量限（LOQ）值分别为 0.13-3.13μg/kg 和 0.25-6.25μg/kg。该经过验证的方法成功地应用于橄榄油和实际精制及使用过的食用油参考材料中 PAHs 的测定。
