Liu Xiaofang, Zhou Shu, Zhu Quanfei, Ye Yong, Chen Huaixia
Hubei Collaborative Innovation Center for Advanced Organic Chemical Materials, Ministry-of-Education Key Laboratory for the Synthesis and Application of Organic Functional Molecules, Wuhan 430062, China.
Hubei Collaborative Innovation Center for Advanced Organic Chemical Materials, Ministry-of-Education Key Laboratory for the Synthesis and Application of Organic Functional Molecules, Wuhan 430062, China
J Chromatogr Sci. 2014 Sep;52(8):932-7. doi: 10.1093/chromsci/bmt119. Epub 2013 Aug 4.
A sample pretreatment method, solid-phase extraction combined with dispersive liquid-liquid microextraction (SPE-DLLME), was established for the sensitive determination of polycyclic aromatic hydrocarbons (PAHs) in smoked bacon samples. In the SPE-DLLME process, three PAHs including naphthalene (Naph), phenanthrene (Phen) and pyrene (Pyr) were extracted from samples and transferred into C18 SPE cartridge. The target analytes were subsequently eluted with 1.2 ml of acetonitrile-dichloromethane (5:1, v/v) mixture solution. The eluent was injected directly into the 5.0 ml ultrapure water in the subsequent DLLME procedure. The sedimented phase was concentrated under a gentle nitrogen flow to 120.0 µl. Finally, the analytes in the extraction solvent were determined by high-performance liquid chromatography with a ultra-violet detector. Some important extraction parameters affecting the performance, such as the sample solution flow rate, breakthrough volume, salt addition as well as the type and volume of the elution solvent were optimized. The developed method provided an ultra enrichment factors for PAHs ranged from 3478 to 3824. The method was applied for the selective extraction and sensitive determination of PAHs in smoked bacon samples. The limits of detection (S/N = 3) were 0.05, 0.01, 0.02 μg kg(-1) for Naph, Phen, Pyr, respectively.
建立了一种样品预处理方法——固相萃取结合分散液液微萃取（SPE-DLLME），用于灵敏测定烟熏培根样品中的多环芳烃（PAHs）。在SPE-DLLME过程中，从样品中提取萘（Naph）、菲（Phen）和芘（Pyr）这三种PAHs，并转移至C18固相萃取柱中。随后用1.2 ml乙腈-二氯甲烷（5:1，v/v）混合溶液洗脱目标分析物。在后续的分散液液微萃取步骤中，将洗脱液直接注入5.0 ml超纯水中。在平缓氮气流下将沉淀相浓缩至120.0 μl。最后，采用配有紫外检测器的高效液相色谱法测定萃取溶剂中的分析物。对影响性能的一些重要萃取参数进行了优化，如样品溶液流速、穿透体积、加盐量以及洗脱溶剂的类型和体积。所建立的方法为PAHs提供了3478至3824的超富集因子。该方法用于烟熏培根样品中PAHs的选择性萃取和灵敏测定。萘、菲、芘的检测限（S/N = 3）分别为0.05、0.01、0.02 μg kg⁻¹。
