Low-temperature cleanup with solid-phase extraction for the determination of polycyclic aromatic hydrocarbons in edible oils by reversed phase liquid chromatography with fluorescence detection
Low-temperature cleanup with solid-phase extraction for the determination of polycyclic aromatic hydrocarbons in edible oils by reversed phase liquid chromatography with fluorescence detection
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DOI：
10.1016/j.foodchem.2013.05.092
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发表时间：
2013-12-01
期刊：
影响因子：
8.8
通讯作者：
Varanusupakul, Puttaruksa
中科院分区：
文献类型：
--
作者：
Payanan, Thongsuk;Leepipatpiboon, Natchanun;Varanusupakul, Puttaruksa
低温净化是一种简单且经济高效的样品制备技术，可以方便地同时处理多个样品，与固相萃取 (SPE) 净化结合开发，用于通过高效液相色谱荧光检测 (HPLC-FLD) 测定精炼和废食用油样品中的 16 种多环芳烃 (PAH)。用少量有机溶剂提取样品，并通过低温净化去除提取物中的大部分脂质。在 HPLC-FLD 分析之前，使用 SPE 柱进一步净化。当使用乙腈：丙酮 4:1 (v/v) 混合物作为萃取溶剂进行两次萃取，在 -18 ℃ 至 -25 ℃ 之间冷冻 24 小时，然后使用 Alumina-N SPE 小柱进行净化时，实现了低温净化的最佳萃取。 PAH 回收率为 45.9-118.5%，16 种测试的 PAH 的检测限 (LOD) 和定量限 (LOQ) 值分别为 0.13-3.13 μg/kg 和 0.25-6.25 μg/kg。该方法已成功应用于橄榄油标准物质和实际精炼及废食用油样品中PAHs的测定。 (C) 2013 Elsevier Ltd. 保留所有权利。
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 degrees C and -25 degrees 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 mu g/kg and 0.25-6.25 mu g/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. (C) 2013 Elsevier Ltd. All rights reserved.