Determination of parent and substituted polycyclic aromatic hydrocarbons in high-fat salmon using a modified QuEChERS extraction, dispersive SPE and GC-MS.
Determination of parent and substituted polycyclic aromatic hydrocarbons in high-fat salmon using a modified QuEChERS extraction, dispersive SPE and GC-MS.
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DOI：
10.1021/jf201745a
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发表时间：
2011-08-10
影响因子：
6.1
通讯作者：
Anderson KA
中科院分区：
文献类型：
--
作者：
Forsberg ND;Wilson GR;Anderson KA
一种快速、简单的改良 QuEChERS（快速、简单、便宜、坚固且安全）提取方法已开发出来并经过验证，可用于测定高脂肪熏鲑鱼中的 33 种母体和取代多环芳烃 (PAH)，与传统 QuEChERS 程序相比，该方法大大提高了分析物回收率。样品处理包括将 PAH 萃取到乙酸乙酯、丙酮和异辛烷溶液中，然后使用分散 SPE 进行净化，并在 SIM 模式下通过 GC-MS 进行分析。在三种市售烟熏鲑鱼（脂肪含量为 3 – 11%）中通过加标回收实验（500 ng/g 湿重）评估方法性能。与传统方法相比，一些 2、3 和 5 环 PAH 的回收率提高了 50 - 200%，而所有 PAH 的平均回收率提高了 67%。方法精密度良好，重复提取通常产生的相对标准偏差 < 10%，检测限在较低的 ng/g 范围内。通过这种方法，单个分析人员可以在 8 小时工作日内提取和净化 ≥ 60 个样品进行 PAH 分析。
A fast and easy modified QuEChERS (quick, easy, cheap, rugged and safe) extraction method has been developed and validated for determination of 33 parent and substituted polycyclic aromatic hydrocarbons (PAHs) in high-fat smoked salmon that greatly enhances analyte recovery compared to traditional QuEChERS procedures. Sample processing includes extraction of PAHs into a solution of ethyl acetate, acetone and iso-octane followed by cleanup with dispersive SPE and analysis by GC-MS in SIM mode. Method performance was assessed in spike recovery experiments (500 ng/g wet weight) in three commercially available smoked salmon with 3 – 11% fat. Recoveries of some 2, 3 and 5-ring PAHs were improved 50 – 200% over traditional methods, while average recovery across all PAHs was improved 67%. Method precision was good with replicate extractions typically yielding relative standard deviations < 10% and detection limits were in the low ng/g range. With this method, a single analyst could extract and cleanup ≥ 60 samples for PAH analysis in an 8 hour work day.
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