Multi-class determination of undesirables in aquaculture samples by gas chromatography/tandem mass spectrometry with atmospheric pressure chemical ionization: A novel approach for polycyclic aromatic hydrocarbons.
Multi-class determination of undesirables in aquaculture samples by gas chromatography/tandem mass spectrometry with atmospheric pressure chemical ionization: A novel approach for polycyclic aromatic hydrocarbons.
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DOI：
10.1016/j.talanta.2017.05.025
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发表时间：
2017-09
期刊：
影响因子：
6.1
通讯作者：
T. Portolés;B. Garlito;J. Nácher-Mestre;M. Berntssen;J. Pérez‐Sánchez
中科院分区：
文献类型：
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作者：
T. Portolés;B. Garlito;J. Nácher-Mestre;M. Berntssen;J. Pérez‐Sánchez
本文建立了一种气相色谱-三重四极杆串联质谱联用（GC-APCI-MS/MS）分析鱼类组织、饲料和饲料原料等19种基质中24种多环芳烃的方法。该方法是基于无缓冲的QuEChERS方法的改进，使用冷冻作为额外的清理步骤，并对最终提取物施加20倍的稀释系数。该程序还测试了15种农药和7种多氯联苯（PCB）同源物，以扩大该方法的范围。GC-APCI-MS/MS具有良好的灵敏度和选择性，可对所有19种基质进行稀释和定量。在2、5和50 ng g−1的峰值水平下对该方法进行了评价。大多数化合物的loq为2 ng g−1，lod范围为0.5 ~ 2 ng g−1。对实际样品的分析显示存在萘、芴、菲、氟蒽和芘，其浓度水平从4.8至187 ng g - 1不等。在鲑鱼和海鲷鱼片中未发现多氯联苯、滴滴涕和杀虫剂。
In this work, a method for the analysis of 24 PAHs in 19 different matrices, including fish tissues, feeds and feed ingredients, has been developed using gas chromatography coupled to triple quadrupole tandem mass spectrometry with atmospheric pressure chemical ionization source (GC-APCI-MS/MS). The method is based on a modification of the unbuffered QuEChERS method, using freezing as an additional clean-up step and applying a 20-fold dilution factor to the final extract. The procedure was also tested for 15 pesticides and 7 polychlorinated biphenyl (PCB) congeners in order to widen the scope of the method.The excellent sensitivity and selectivity provided by GC-APCI-MS/MS allowed the dilution of the sample extracts and quantification using calibration with standards in solvent for all the 19 matrices tested. The developed method was evaluated at 2, 5 and 50 ng g−1spiking levels. LOQs were 2 ng g−1for most compounds, and LODs ranged from 0.5 to 2 ng g−1.Analysis of real-world samples revealed the presence of naphthalene, fluorene, phenanthrene, fluoranthene and pyrene at concentration levels ranging from 4.8 to 187 ng g−1. No PCBs, DDTs and pesticides were found in fillets from salmon and sea bream.