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Single laboratory validation of an environmentally friendly single extraction and cleanup method for quantitative determination of four priority polycyclic aromatic hydrocarbons in edible oils and fats

机译:单实验室验证了一种环保的单一萃取和净化方法,用于定量测定食用油脂中的四种优先多环芳烃

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This paper reports a simple, rapid, reliable and environmentally friendly gas chromatography-mass spectrometry (GC-MS) method for analyzing polycyclic aromatic hydrocarbons (PAHs) in edible oils and fats. The fat sample was first dissolved in acetonitrile while oils were loaded directly onto a solid phase extraction cartridge. PAHs were eluted with acetonitrile. Owing to the background interference, GC-MS was found to be applicable for 4 European Union (EU) priority PAHs (benzo[a]pyrene, benz[a]anthracene, benzo[b] fluoranthene and chrysene) in various types of edible oils and fats, but not for 15+1 EU-priority PAHs. An adequate linear relationship was obtained in the studied concentration range (0.1-60.0 mu g kg(-1)) in samples; analytical limits of detection and quantification were 0.1 and 0.25 mu g kg(-1), respectively. Due to the lack of a certified reference material, spiked recovery and a FAPAS quality control material were employed to assess the accuracy. The mean spiked recoveries for 4 PAHs, studied at concentration levels of 0.25 (method limit of quantification (MLOQ)), 1.0 and 2.0 mu g kg(-1), ranged from 86 to 114%. Precision values, expressed as relative standard deviation, were below 10% at aforementioned spiking levels. Extraction and cleanup of a batch of 20 samples can be completed within an hour by one worker. The developed method was successfully applied for the PAH determination in real commercial samples, including lard, olive, corn, peanut, sunflower seed, rapeseed, sesame and vegetable oil.
机译:本文报道了一种用于分析食用油脂中多环芳烃(PAHs)的简单,快速,可靠和环保的气相色谱-质谱(GC-MS)方法。首先将脂肪样品溶解在乙腈中,同时将油直接加载到固相萃取柱上。 PAHs用乙腈洗脱。由于背景干扰,发现GC-MS适用于各种食用油中的4种欧盟(EU)优先多环芳烃(苯并[a] [,苯并[a]蒽,苯并[b]荧蒽和)和脂肪,但不适用于15 + 1欧盟优先PAH。在样品的研究浓度范围(0.1-60.0μg kg(-1))中获得了足够的线性关系;检测和定量的分析极限分别为0.1和0.25μg kg(-1)。由于缺少经过认证的参考材料,因此采用加标回收率和FAPAS质量控制材料来评估准确性。在浓度水平0.25(定量方法(MLOQ)),1.0和2.0μg kg(-1)浓度范围内研究的4种PAH的平均加标回收率在86%至114%之间。在上述加标水平下,以相对标准偏差表示的精度值低于10%。一个工人可以在一小时内完成一批20个样品的提取和净化。该方法成功地用于猪油,橄榄,玉米,花生,葵花籽,油菜籽,芝麻和植物油等实际商业样品中的PAH测定。

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