A validated liquid chromatographic method for the determination of polycyclic aromatic hydrocarbons in honey after homogeneous liquid-liquid extraction using hydrophilic acetonitrile and sodium chloride as mass separating agent
A validated liquid chromatographic method for the determination of polycyclic aromatic hydrocarbons in honey after homogeneous liquid-liquid extraction using hydrophilic acetonitrile and sodium chloride as mass separating agent
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DOI：
10.1016/j.chroma.2014.12.039
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发表时间：
2015-01-16
影响因子：
4.1
通讯作者：
Fytianos, Konstantinos
中科院分区：
文献类型：
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作者：
Koltsakidou, Anastasia;Zacharis, Constantinos K.;Fytianos, Konstantinos
在本报告中，提出了一种简单和经济有效的方法，用于测定12个美国环保局优先多环芳烃（PAHs）的蜂蜜样品后，盐辅助液-液萃取和超高效液相色谱荧光检测。样品处理是基于使用亲水性乙腈作为萃取溶剂，并在高盐度条件下进行相分离。由于样品的高糖含量，相分离毫不费力地得到促进。对蜂蜜样品浓度、提取溶剂的种类和体积、无机盐的种类和用量、提取时间和离心时间等因素对提取效率和方法灵敏度的影响进行了系统研究。根据委员会决议2002/657/EC指南，对该方法进行了内部验证。该方法的检测限（LOD）在0.02和0.04 ng mL（-1）之间（相当于0.08和0.16 ng g（-1）），接近欧洲法规（EC）836/2011关于食品中多环芳烃的质量标准。所有加标水平的平均分析偏倚（表示为相对回收率）在54-118%范围内可接受，而相对标准偏差（RSD）低于19%。所提出的方法已满意地应用于分析选定的多环芳烃残留在各种蜂蜜样品从希腊地区。(C)2014爱思唯尔有限公司版权所有。
In the present report, a simple and cost-effective method for the determination of twelve US EPA priority polycyclic aromatic hydrocarbons (PAHs) in honey samples after salting-assisted liquid-liquid extraction and UHPLC with fluorescence detection is proposed. The sample treatment is based on the usage of hydrophilic acetonitrile as extraction solvent and its phase separation under high salinity conditions. Due to the high sugar content of the samples the phase separation is promoted effortlessly. Several parameters affecting the extraction efficiency and method sensitivity including the concentration of the honey samples, the type and volume of the extraction solvent, the type and quantity of the inorganic salt, extraction time and centrifugation time was systematically investigated. The method was validated in-house according to the Commission Decision 2002/657/EC guidelines. The limit of detection (LOD) of the method lay between 0.02 and 0.04 ng mL(-1) (corresponding to 0.08 and 0.16 ng g(-1)) which are close to the quality criteria established by European Regulation (EC) 836/2011 concerning the PAHs in foodstuffs. The mean analytical bias (expressed as relative recoveries) in all spiking levels was acceptable being in the range of 54-118% while the relative standard deviation (RSD) was lower than 19%. The proposed method has been satisfactorily applied for the analysis of the selected PAHs residues in various honey samples obtained from Greek region. (C) 2014 Elsevier B.V. All rights reserved.