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采用 QuEChERS 萃取和气相色谱-串联质谱法测定食用海鲜中的多环芳烃。

Determination of polycyclic aromatic hydrocarbons in edible seafood by QuEChERS-based extraction and gas chromatography-tandem mass spectrometry.

机构信息

Laboratory Services Div, Minnesota Dept of Agriculture, 601 North Robert St, St Paul, MN 55155, USA.

出版信息

J Food Sci. 2012 Jul;77(7):T131-7. doi: 10.1111/j.1750-3841.2012.02758.x. Epub 2012 Jun 1.

Abstract

UNLABELLED

A high-throughput analysis of polycyclic aromatic hydrocarbons (PAHs) in edible seafood using QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) based extraction and gas chromatography-tandem mass spectrometry (GC-MS/MS) was developed and validated in 4 seafood matrices--crab, finfish, oyster, and shrimp. The extraction employs QuEChERS with dispersive solid phase extraction (dSPE) using cleanup sorbent that includes C18. The acetonitrile extract is partitioned into hexane and analyzed by GC-MS/MS. The procedure was validated by spike recovery experiments of 15 parent and 5 substituted PAHs at 5ppb and 25 ppb levels in the 4 matrices. Recoveries were 71%-130% with RSDs less than 14%. The limit of quantitation (LOQ) for benzo[a]pyrene are 0.4-2.5 ppb depending on matrix. For all 15 parent PAHs the LOQs are less than 10% of the Levels of Concern established by the U.S. Food and Drug Administration. Good recoveries were also achieved in aged spikes at 5 ppb level in oyster and shrimp. Method accuracy was further evaluated by analyzing NIST Standard Reference Material 1974b. Ten of 14 incurred PAHs corresponding to the parent compounds in the present study fell within the control limits established by the National Oceanic and Atmospheric Administration. Using the present method approximately 20 samples every 24 h can be analyzed with confirmation.

PRACTICAL APPLICATION

The presented analytical method could be used for seafood safety assessments to examine petroleum contaminant levels in edible seafood after an oil spill. The method is fast and sensitive.

摘要

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使用 QuEChERS(快速、简单、廉价、有效、坚固、安全)基于提取和气相色谱-串联质谱法(GC-MS/MS)对食用海鲜中的多环芳烃(PAHs)进行高通量分析,并在 4 种海鲜基质——蟹、鱼、牡蛎和虾中进行了验证。该提取方法采用 QuEChERS 与分散固相萃取(dSPE)相结合,使用包括 C18 的净化吸附剂。乙腈提取物被分成正己烷和通过 GC-MS/MS 进行分析。该程序通过在 4 种基质中以 5ppb 和 25ppb 水平在 15 种母体和 5 种取代 PAHs 的加标回收实验进行验证。回收率为 71%-130%,RSD 小于 14%。取决于基质,苯并[a]芘的定量限(LOQ)为 0.4-2.5ppb。对于所有 15 种母体 PAHs,LOQs 均小于美国食品和药物管理局规定的关注水平的 10%。在牡蛎和虾中,在 5ppb 水平的老化加标中也获得了良好的回收率。通过分析 NIST 标准参考物质 1974b 进一步评估了方法的准确性。在本研究中,与母体化合物相对应的 10 种 14 种实际发生的 PAHs 落在国家海洋和大气管理局建立的控制限内。使用本方法,每 24 小时大约可以分析 20 个样品,并进行确证。

实际应用

所提出的分析方法可用于海鲜安全性评估,以检查溢油后食用海鲜中的石油污染物水平。该方法快速灵敏。

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