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固相萃取-高效液相色谱联用测定食用油中的4种多环芳烃 |
Determination of four polycyclic aromatic hydrocarbons in edible oil by solid-phase extraction coupled with high performance liquid chromatography |
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DOI: |
中文关键词: 食用油 多环芳烃 测定 固相萃取 高效液相色谱-荧光检测 |
英文关键词:edible oil polycyclic aromatic hydro carbons (PAHs) determination solid-phase extraction high performance liquid chromatogra phy-fluorescence detection |
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中文摘要: |
采用固相萃取与高效液相色谱-荧光检测联用技术,建立了食用油中4种多环芳烃(PAHs),即屈(Chr)、苯并(a)蒽(BaA)、苯并(b)荧蒽(BbF)和苯并(a)芘(BaP)的快速分析方法。自制固相萃取小柱,并优化了固相萃取条件。结果表明,食用油样品经异丙醇稀释后可直接进行固相萃取分析。固相萃取优化条件为:Benzo Ⅱ SPE填料1.0 g,洗脱液丙酮8 mL,清洗液异丙醇4 mL,上样液为2 mL 0.2 g/mL的异丙醇稀释油样。4种PAHs 在1~50 ng/mL(苯并(b)荧蒽为2~50 ng/mL)质量浓度范围内具有良好的线性关系,相关系数在0.999 2~0.999 8之间,检出限为0.14~0.76 ng/g,日内、日间相对标准偏差在2.7%~9.9%之间。对中国计量科学研究院提供的3份橄榄油样品PAHs测定的结果与所给参考值(1号油样BaP含量)相差10.3%。建立的方法可用于多种食用油中4种PAHs的分析检测,具有耗时短、有机溶剂消耗少、简便快速等优点。 |
英文摘要: |
A rapid method for the determination of four polycyclic aromatic hydrocarbons (PAHs)(Chr,BaA,BbF and BaP) in edible oil was developed by solid-phase extraction coupled with high performance liquid chromatography-fluorescence detection (HPLC-FLD).The solid-phase extraction column was self-made and the solid-phase extraction conditions were optimized.The results showed that the edible oil sample could be analyzed directly by solid-phase extraction after it was diluted in isopropanol. The optimal solid-phase extraction conditions were obtained as follows:1.0 g Benzo Ⅱ SPE,with 8 mL acetone as desorption solvent,4 mL isopropanol as washing solvent,2 mL 0.2 g/mL isopropanol diluted oil. The linearity range,correlation coefficient,the limit of detection and relative standard deviation of the proposed method were 1-50 ng/mL(2-50 ng/mL for BbF),0.999 2-0.999 8,0.14-0.76 ng/g and 2.7%-9.9%.The relative error between determined value and reference value of BaP in three kinds of olive oils provided by National Institute of Metrology in China was 10.3%. The established method had the items of short time,small consumption of organic solvent and simpleness,which was suitable for the determi nation of four PAHs in edible oils. |
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